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VOLUME 49 l Summer Edition, 2016 | Environmental Health Ongoing drought situation in several parts of country reiterates and reminds us of our humungous responsibility as an individual, to commit sincerely to cause of water sustainability, conservation and held ourselves accountable to environment and society we live in. As 76 million people in India don’t have access to safe water. There are numerous water conservation tips, it all starts with you. IT’S WATER USE IT WISELY #BeWaterWise #WaterForAll #BeAWiseGardner Environment | Textile | Pharma

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Page 1: IT’S WATER · content in different food samples such as grains, fruits, vegetables, water, cereals, milk, dairy prod-ucts, herbal products, edible oils, honey, beverages and spices

VOLUME 49 • Summer Edition, 2016

VOLUME 49 l Summer Edition, 2016 | Environmental Health

Ongoing drought situation in several partsof country reiterates and reminds us of ourhumungous responsibility as an individual, tocommit sincerely to cause of water sustainability,conservation and held ourselves accountable toenvironment and society we live in.

As 76 million people in India don’t have access to safe water.

There are numerous water conservation tips, it all starts with you.

IT’S WATER USE IT WISELY

#BeWaterWise #WaterForAll #BeAWiseGardner

Environment | Textile | Pharma

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WHAT’S

Freshinside...

Customer First: Success Story

• ARBRO,marketleaderinfoodtestingrelieson PerkinElmer’sICPMS ....................................... 3-4

Featured Article

• Detectionandidentificationofmicroplasticsin cosmeticformulationsusingIRMicroscopy ............. 5-7

Application Focus

• TGAandIRhyphenationappliedtoroutineanalysis of components used in electronic circuits ............... 8-9

Environment Focus

• MeasurementandanalysisofAgnanoparticlesinwastewaterusingSP-ICPMS .............................. 12-13

• Analysisofmineralsindrinkingwaterusing Flame AA ........................................................... 14-16

Textiles

•PVCscreeningintextileindustryusingFTIR ........ 17-18

•AnalysisoforganotoxinsintextilesusingGCMS ......19•Determinationofextractablemetalsintextiles usingICPMS.............................................................20

Pharmaceuticals

•ImplementationofUSP<232><233>using

ICP-OES/MS ....................................................... 21-23•ImplementationofUSP<857>usingLambda 365UV-VisspectrophotometerandUOQkit ...... 24-25

•Determinationofcholesterollevelinhuman serumbyUV-Visspectrophotometer .................. 26-27

Expanding food testing capabilities further

•PerkinElmeracquiresPerteninstruments ...................28

News and Event Update

AsiaPharmaandDTGexhibitions-Bangladesh .............29IAIA seminar series .......................................................29ICEFN-NainitalandICNANO-Bangaloreconferences .....29NCL-PuneandPU-Chandigarhworkshops ....................30EnhancingAnalyticalCapabilities

seminar-Visakhapatnam ..............................................30

ThanksfordownloadingFresh49,SummerEdition!

Occurenceofevents-worldconference-COP21,ongoingdroughtsituation,ourowncapital’strystwithoddevenrule,NGTseekingbanonuseofmicroplastics,PMNarendraModilayingemphasisoncleandrinkingwater,hasonceagainplacedenvironmenttopriorityfocusarea,whichindeedshouldbe,keepingwiththatwehavededicated beginning sections of this edition to environment with textileandpharmainsubsequentsections.

WewouldliketothanksArbroteamforsharingtheirexperiencewith our application and service team as they continue to use our ICPMSforfoodcontaminants.

Through this edition of Fresh we are very pleased to introduce PertenInstrumentsinourfoodtestingportfolio,therebyexpandingcapabilities to assist our customers in addressing rigorous regula-tionsforfoodqualitycontrol.

As you must be aware of that we are engaged in customer satis-factionsurveythroughourpartners“MarketInsightConsultants”,sincerethanksforyourfeedback,beingaresponsibleorganizationwe are trying to implement your suggestions to serve you better andrequesttokindlyobligewithmoreenthusiasticresponse.WewouldreallyappreciateyourfeedbackonthiseditionofFreshalso, as we continuously thrive to introduce new sections and more informative content.

With anticipation that you will enjoy reading Fresh, we wish you all safeandhealthylivinginsummer!

Sincerely PerkinElmer India

Dear customers,

AmessagefromteamPerkinElmer,EnvironmentHealth....

Table of Contents

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IntroductionTheFoodSafetyandStandardsAuthor-ityofIndia(FSSAI)hasbeenestablishedundertheFoodSafetyandStandardsAct, 2006 which consolidates various acts & orders that have, up till now, handled food related issues in various MinistriesandDepartments.FSSAIwascreated for developing and upholding science based standards for articles of food and to regulate their manufacture, storage, distribution, sale and import to ensure safe and wholesome food is available for human consumption. The Act also aims to establish a single reference point for all matters relating to food safety and standards, by moving from multi- level, multi- departmental control to a single line of command. To this effect, the Act establishes an inde-pendent statutory Authority – the Food SafetyandStandardsAuthorityofIndia,headquarteredinDelhi.FoodSafetyandStandardsAuthorityofIndia(FSSAI)andtheStateFoodSafetyAuthoritiesshallenforce various provisions of the Act.

ARBRO Pharmaceuticals Ltd., Analytical DivisionARBROisamulti-disciplinarycontractresearchorganizationandfoodtestinglabinIndia.ARBROAnalyticalDivisionwasestablishedin1990inNewDelhi.Subsequently,twoadditionalstateofthe art laboratories were added one in BaddiandanotherinBangalore.Theyspecializeinpharmaceuticaltesting,food testing, herbal testing, water test-ingandmore.ARBROoffersanalyticalmethod development, method valida-tion, stability testing, product testing, product development, chemical testing and microbiology testing lab services

along with pre-shipment inspection. They are one of the largest food testing labsinIndia,accreditedbyNABLasperISO/IEC17025andauthorizedbyFSSAIforchemicalandbiologicaltest-ing of food, beverages and agricultural products.Havingmorethan20yearsofexperienceasafoodtestinglab,ARBROoffers a single point solution to all the food testing needs of the industry for bothdomesticandexportmarkets.Theyhave a team of over 300 professionals backedbyanultramodernfoodtestinglab infrastructure and state of the art equipment.Theyanalyzefoods&agri-culturalproductsasperFSSAI,BIS,EIC/EIA,APEDA&European(EU)standardsandFSSA(FoodSafetyandStandardsAct).Thetestingcarriedoutcompliestonational and international standards us-ing globally acceptable methods laid out byAOAC,ASTA,AOCS,CODEX,PFA,BIS,EUandUSFDA.

Investment in ICP-MS A critical component of ARBRO’s mission is to determine heavy metal content in different food samples such as grains, fruits, vegetables, water, cereals, milk, dairy prod-ucts, herbal products, edible oils, honey, beverages and spices. They were looking for a fast throughput analytical tool or instrument to meet their demand of over 50 samples per day to determine heavy metal content to meet various regulations including FSSAI and AOAC. Seven years ago, they decided to invest in the PerkinElmer ELAN ICP-MS model DRC- e. The criteria for selecting this unitwasitsuniquereactionandcollisioncell technology, rugged unit, less user

maintenance, local support, long term stabilityandprecision.TheELANICP-MShasbecomeanintegralpartofARBRO’stestingforvariousfoodsamples.Beforetheyinvestedinthistechnique,theyadoptedothermethodslikeAASwithgraphitefurnaceandICP-OES.UsingtheICP-MS,theyareabletoanalyze10-20 times as many samples per day astheydidbefore.ARBROsays,‘thePerkinElmerinstrumentsarethemostimportantpiecesofequipmentweown,particularly to help us conform to vari-ousregulationslikeFSSAIandAOACforthe determination of metal impurities likelead,cadmium,arsenic,mercury,selenium,tin,copper,zinc,nickelandchromium.’

AtypicalICP-MSanalysisforafewsampleswascarriedasperARBRO’sstandard internal protocols and vali-datedmethodsaslaidoutbytheAOAC.Samplesofhoneyandricewereana-lysedforheavymetalslikearsenic,leadandcadmiumusingthePerkinElmerELANDRC-eICP-MS.

HoneyApproximately1gmofhoneywastakeninavolumetricflaskand5mlofSu-pra pure grade nitric acid was added. Digestionwascarriedoutonahotplateuntil brown fumes were no longer seen. After cooling to room temperature, the volume was increased up to 50ml with deionizedwaterandaspiratedintothespectrometer.

RiceSameprocedureashoney,butapproxi-mately double the amount of sample was digested each time.

ARBRO, market leader in food testing, is cracking down on food contaminants using PerkinElmer’s ICPMS

Customer Success Story

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Sample As (ppb) Pb (ppb) Cd (ppb)

Honey-1 56.379 24.777 1.385

Honey-2 60.831 15.875 1.484

Honey-3 58.717 27.190 1.462

Honey-4 58.381 16.015 1.068

FSSAI

Limit

1100 2500 1500

EICLimit 250 1000

Results

Rice

Sample As (ppb) Pb (ppb) Cd (ppb)

Rice-1 65.343 7.515 7.737

Rice-2 34.169 3.226 4.888

Rice-3 21.963 1.657 3.413

FSSAI

Limit

1100 2500 1500

EICLimit 200 200

ConclusionIn all samples, the levels of heavy metals were far below the limits specified by FSSAIandEIC.

Analytical Solutions:Forthelastsevenyears,ARBROhasana-lyzedvariousfoodsampleslikehoney,milk,cheese,namkeen,cookedfoods,beverages,juiceandwaterusingaPerki-nElmerICP-MS.BeingaNABLaccreditedlab,ARBROarereceivingsamplesfromdifferent parts of the country to comply withFSSAIregulations.Theyarefollow-ing various global standard methods as mentionedabovetoanalyzethesefoodmatrices. They have a team of chemists and scientists to develop and validate ro-bustmethods,checkaccuracy,precisionand recovery. These data produced can also be used in the court of law. Today, ARBROhasanalyzedmorethan50,000samples catering to different clients throughout the globe.

ARBROisaverycustomerfocusedorganizationduetotheirqualityserviceand loyalty to their clients and have grown multi fold over the last 10 years. Today,ARBROhasbecomeoneofthelargestfoodtestinglabsinIndia.ByhavinghighqualityanalyticalequipmentlikethePerkinElmerICP-MS,theyareamarketleaderinfoodtesting.

PerkinElmerfeelsproudtobeassociatedwithARBROastheyhaveshownthetrust in this partnership to achieve theirgoals.ARBROhas,‘alwaysfoundthe technical and service support ofPerkinElmeranditspartnerstobenothinglessthanextraordinary.Whether it is a new installation or preventativemaintenance,PerkinElmerservice engineers always conduct themselves in a very professional manner.We’vealsofoundPerkinElmer’stechnical and application support specialiststobeequallyimpressive.’

Thank you, Dr. Saurabh Arora for ac-knowledging PerkinElmer’s support to help ARBRO become one of the highest quality leading global test-ing labs. PerkinElmer looks forward to continue supporting you in the future as you continue to grow.

References:• ARBROwebsitehttps://testing-lab.com/2012/05/arbro-authorized-by-fssai-for-testing-of-food-samples/

• FSSAIwebsitewww.fssai.gov.in/

Food Safety & QualityTo assess the quality and safety of food supplies around the world, we offer industry-leading solutions for characterizing nutritional components within food and agricultural products and detecting risks to human and animal health.

•Detectharmfullevelsoftoxins,heavy metals, and pesticides.

•Ensureaccuratelabelingandcompliance with regulations around the globe.

•Evaluatethequalityofrawma-terials prior to food processing

•Meettargetsfornutritionalcontent.

•Maintainstandardsforflavor,aroma, and consistency in food and beverages.

•Understandhowfoodpackag-ing effects the food it contains.

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VOLUME 49 • Summer Edition, 2016

Detection and Identification of Microplastic Particles in Cosmetic Formulations using IR Microscopy

Featured Article

IntroductionMicroplasticsorMicrobeadsareplasticpiecesorfibreswhichareverysmallinsize,typicallysubmillimeter,measuringlessthan5mm, infact microbeads found in personal care products are almost always smaller than 1mm. These are mainly made of poly-ethylene(PE),butcanalsobemadeofpolypropylene(PP),polyethylenetetrapthalate(PET),polymethylmethacrylate(PMMA)and nylon.

Manycosmeticproducts,suchasfacialscrubs,toothpastes,andshowergels,currentlycontainmicroplasticbeadsasabrasivematerials.Thesemicroplastics,whicharetypicallysubmillimetreinsize,getwasheddownthesinkandaretoosmalltobefilteredbysewagetreatmentplantsconsequentlyendingupintheriversystemsandultimatelyintheoceans,wheretheycon-tributetohugechunkofplasticsoupinenvironment.Thesemicroplasticscanbeingestedbymarineorganismsandfishandendup in the human food chain.

December 2015:Obamasignsbillagainstmicrobeads:theMicrobead-FreeWatersAct

October 2015: Gothenberg(Sweden)bansplasticmicrobeads

September 2015:California(USA)signsacompletebanonuseofmicrobeadswithoutloopholes

July 2015:Canadasignsacompletenationwidebanonuseofmicrobeadsinpersonal care products

March 2016: NGT seeks centre’s response on plea for ban on use of microplastics

NationalGreenTribunalissuednoticestotheUnionHealth,MinistryofEnvironment&ForestandMinistryofWaterResourcesseekingtheircommentsonwhathasbeendone to identify and curb this growing threat of use of microbeads in cosmetic and personal care products in India alleg-ingtheiruseisextremelydangerousforaquaticlifeandenvironment.

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With ongoing international campaign for ban on usage of plastic microbeads and momentum gaining in India also for regulating the use of microbeads in cosmetics, it is now time for Indian manufacturers to equip themselves in advance for addressing this upcoming regulatory change and above all deliver to cause of environmental sustainability.

Author:Ian RobertsonPerkinElmer, Inc.Seer Green, UK

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VOLUME 49 • Summer Edition, 2016

In2014anumberofU.S.statesbannedthe use of microplastics in cosmetic for-mulations and most cosmetic companiesare voluntarily phasing out their use.

Infrared(IR)spectroscopyistheestab-lishedtechniqueforidentifyingpolymermaterialsandhasbeenusedextensivelyfor identifying large (over 100 microm-eter)polymermaterials.TheSpectrumTwo™isaportableFT-IRspectrometerthatcanoperatefromabatterypackand has been used on boats for immedi-ate identification of these polymers.1 Formicroplastics, down to a few microm-etersinsize,anIRmicroscopecanbeused for the detection and identification of these materials.

Two commercially available productsweretestedusingtheSpotlight™200iIRmicroscope system in order to determine whether microplastics were present as theexfoliantandtoidentifythetypesofplastics used.

Product 1 is a commercially availablefacial scrub. Product 2 is a commerciallyavailablebodyscrub.Eachoftheseproductswasmixedwithhotwaterinorder to dissolve the soluble ingredients in the formulation. The resulting solution was filtered through a 50 micrometer mesh, capturing any insoluble compo-nents greater than 50 micrometers in size.ThefilterwasthenallowedtodryinairpriortoIRmicroscopymeasure-ments. The samples were measured both directly on the mesh and also after transferring the residual particles ontoanIRtransmittingwindowonamicroscopeholder.Visibleimagesofthecollected microplastics are shownas Figures 1a and 1b.

Figure 1a: Microplastics in Product 1 (facial scrub) col-lected on mesh.

Figure 1b: Magnified view of microplastics collectedfrom Product 2 (body scrub).

Figure 2: Spectra from a microplastic particle in Product1. Transmission spectrum (black) and reflectancespectrum (red).

Figure 3: The Analyze Image software routine detectsthe particles in Product 1.

It is clear from these images that Product1 has irregular-shaped microplastics with particles of two different colors. The particles from Product 2 are regularspheres with those visible in Figure 1bbeingapproximately50and80microm-eters in diameter. Infrared spectra of these materials can be measured ineither transmission or reflectance on theIRmicroscope.Spectrameasuredononeof the particles in Figure 1a, in-situ onthe mesh, are shown as Figure 2.

The transmission spectrum has a muchhigher signal than the reflectance spec-trum and gives better sensitivity for thismeasurement. In addition, the bandsin the reflectance spectrum are moreintenseduetothefactthattheIRbeamis effectively passing twice through thesample,knownastransflectance.Forsmaller particles this does not cause anyproblems; but for larger particles the path length may be too large leadingtototallyabsorbingbands,thusmakingidentificationmoredifficult.However,inthis case, it would be possible to identifythe material from either the transmissionor reflectance spectrum. The mesh mayinterfere with the transmission measure-ment, slightly decreasing the amountof energy reaching the detector. This

explainsthebaselineslopeobservedinthe spectrum, but it does not significant-ly impact the overall measurement.Toobtainthebestqualityspectrumofthe material, the sample can betransferredontoanIR-transmittingwin-dow material, such as potassium bro-mide(KBr).AKBrwindowwasplacedonto the mesh containing the sampleand the mesh inverted therebytransferring the microplastic particlesdirectlyontotheKBrwindow.

A“VisibleImageSurvey”wascollectedover the area containing the majorityoftheparticlesinProduct1.Selectingthe“AnalyzeImage”functionintheSpectrum10softwareinvokestheintel-ligent automated routine for detectingparticleswithinthisVisibleImageSurvey,whichisdisplayedas“analyzeimageresult”showninFigure3.

This routine will automatically detect anyparticles present in the visible image andmarkthemasregionsofinterest.Itwillthencalculatethemaximumrectangularaperturesizethatcanfitwhollyinsideeachoftheparticles,thusmaximizingsignal-to-noise when the data is scanned. In the past, manual selectionof the regions of interest and setting ofaperturestookaconsiderableamountoftime.Clicking“ScanMarkers”initiatesthe collection of transmission spectra(usingequivalentaperturesforthebackground)foreachparticle,displayingratioed sample spectra in real time asthey are collected. Automatic processing of the spectra, using software routinessuchasSearch,Compare,orVerify,canbe performed during data collection. In

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this case, the analysis of the microplas-tics, a spectral search was performedagainst a library of polymer spectra togive the identity of each of the particlesas shown in the results screen in Figure 4.

Figure 4. Results screen for the detection and identifi-cation of particles.

Figure 5: Top – spectrum of polypropylene in Product1. Middle – spectrum of polyethylene in Product 1. Bottom – spectrum of polyethylene in Product 2.

The results show that Product 1 hastwo different types of polymers present,

SummaryMicroplasticsareamajorconcernregarding their impact on the environ-ment and as such their use in consumerproducts is increasingly being prohibited.AnautomatedIRmicroscopysystemhasbeen shown to be an invaluable methodfor the detection and identification ofa source of microplastics in cosmeticformulations.TheworkpresentedherewillbeextendedtoanalyzesamplesofmicroplasticscollectedfromEuropeanriver systems to illustrate how wide-spread this pollution problem is withinmarine environments.

References:• http://www.beatthemicrobead.org/en/results• http://www.thehindu.com/news/cities/Delhi/national-green-tribunal-seeks-centres-response-on-ban-of-microplastics/article8379260.ece•http://timesofindia.indiatimes.com/home/environment/pollution/NGT-seeks-Centres-response-on-plea-for-ban-on-micro-plastics/article-show/51383268.cms

polypropylene and polyethylene. Product2 contains only particles of polyethylene.RepresentativespectraareshowninFigure5.Smalldifferencesareobserv-able in the spectra of the polyethylenebetween the two different products,mostlikelyduetoadditivespresent.

IR Microscopy that addresses your increasingly challenging samples!

Spotlight™ 150i/200i FTIR Microscope Systems

•Bothmicroandmacrosamplingversatility•Smartandintelligentregion-of-interest(ROI)search•AutoATRsetupandapertureoptimizationforfast,

accurate results• Inbuiltstepwiseworkflowthatmakessetup,scanningand

analysis simple and straightforward•Batchanalysisandreportingformultipointand

multicomponent measurement•Configurablevalidationroutines•Simplifieddatacollection,processingandanalysisusingSpectrum™ 10 software

Materials | Pharmaceuticals | Academic Research | Forensics | Biomedical | Biomaterials

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IntroductionFailure of electronic circuits is often causedbytheadverseeffectsofexces-sive heat buildup. Thermal analysis techniqueshavelongbeenappliedtoquantifytheeffectofelevatedtempera-tureoncomponentexpansion,reactiv-ity, and mass loss. A new tool in this familyoftechniquesistheTGA8000™ interfacedtootheranalyzersforevolvedgasanalysis(Figure1).

TheTGA8000,withtheSpectrumTwo™ FT-IRandTL8000interfacecontroller,hasseveralnewfeaturesthatmakeitespecially applicable for routine analysis of components used in the electron-ics industry. These features include improved baseline and purge control characteristics, and a patent-pending autosampler. Furthermore, the interface to the infrared spectrometer features a heated valve and other features that allow it to be easily switched in and out ofthelineinordertomakeitconveni-enttoanalyzetheevolvingdegradationproducts.Primarily,thekeytoperfor-mance is a balance-and-furnace system designed for measuring small changes in weight over time and temperature.

TGA and IR hyphenation applied to routine analysis of components used in electronic circuits

Application focus

Authors:Bruce CasselSaurabh PatelPerkinElmer, Inc.Shelton, CT

Figure 1. TGA 8000, TL 8000 interface and Spectrum Two FT-IR.

TGA 8000: Keys to PerformanceHigh SensitivityOneoftheprimaryrequirementsofelec-tronic circuit and housing components is that they are stable over time even when subjected to somewhat elevated temperatures. When detecting the loss of mass over time it is necessary to havethehighestsensitivityinordertoquan-tify small changes in weight, since these volatiles may find their way into sensitivecomponents.Detectinglowlevelsofvolatilesaccuratelyrequiresastable,flat,reproducible baseline, against which the mass loss is measured. Figure 2 shows severalcomponentsextractedfromafailed smart phone that was dissem-bledandanalyzed.Thetemperatureprogram is the same as that used for thedelaminationtestforPCBmateri-als.1 The Y-scale shows the weight loss of the first 2.5% of weight under these rateaccelerated conditions using samples of a few up to 20 mg of sample for

analysis. Also shown on a weight Y-scale is a no-sample baseline, stable within a few micrograms - although no baseline was subtracted from the data displayed. As part of product verification testing in manufacturing, the baseline must pass rigid tests of reproducibility and drift of within 10 µg when heated between 50°Cand1000°C.

Figure 2. Volatile losses of smart phone components (PCB, pc chip, gorilla glass, polycarbonate case mate-rial, and flexible connectors).

Temperature Control and AccuracyTheTGA8000canbecalibratedsuchthat the temperature of the sample is accuratewithin1°Coverarangeofeating and cooling rates and when held isothermally. This capability is especially important for the reliability of isother-mal stability testing. The use of a closely coupled, low mass furnace facilitates rapidequilibriumandcool-downrates.For even faster cool-down times a water cooled furnace accessory is available.

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mation on the mechanisms of thermal degradation. This evolved gas analysis is compatible with the thermogravimetric analyzer(TGA)autosamplerandcanbeincorporated at a later date, if the need arises. Additionally, to enable detection oftracelevelimpuritiestheTGAcaninterface with gas chromatography or mass spectrometry with the aid of the TL8000.

Figure 3. PerkinElmer’s TimeBase software screen as displayed after TG-FT-IR analysis. Bottom pane: Absorption versus temperature as solder paste sample is heated in nitrogen. The vertical line can be placed anywhere along the curve to display the IR spectrum at that time or temperature. Top pane: The absorptionspectrum at 155.4°C. A gas phase spectral library identified the component evolving at that temperature as Phenylmethanol.

Automated TestingTheTGA8000nowincorporatesanew-ly designed and patented autosampler with a 48-sample carousel. This system features improved reliability and ease of use of sample handling that will be ap-preciated even if the sample throughput isnotexpectedtobegreat.Anautosa-mpler facilitates fully automated testing,including automated run-time weighing, optional run-time capsule opening, and routinesforoptimizing,calculating,andtesting the data using the powerful Pyris™ Player software.

Sample Atmosphere ControlPurge streams are controlled with preci-sion mass-flow controllers which are pre-calibrated to common gas types, so that only the desired gas type and flow rate need selecting. The applied run-time gas flow rates are stored with the data versus time and temperature to later confirm the gas flow changes have beenexecutedasspecifiedbythetestprotocol.Forexample,arapidnitrogenpurge at the start of the analysis can en-surethatoxygenfromincursionduringsampleloadinghasbeenexpelledbeforeapyrolysis.TheGMD8000gasmixingaccessory is also available for multi-gas mixingandmoreadvancedprogram-mingrequirements.Thesmallfurnaceenclosure volume means that purge gas switchoverbetweenoxidativeandinertatmospheres is rapid, thus reducing thetimerequiredtopurgeoutoxygenintroduced when the sample is loaded. TheTGA8000isasealedsystem,whichmeansthatoxygenisexcludedonceithas been purged out from loading.

Evolved Gas Analysis using Infrared SpectroscopyTheTL8000interfacetoaspectrometerfeatures a new purge system to mini-mizethedetectionofwatermoistureandCO2 from the lab atmosphere. This enables the detection of lower levels of waterandCO2 coming off the sample, which together with identification of epoxy,phenolic,adhesive,andsolderpaste products, can give useful infor-

ConclusionWhethertheneedistoquantifycar-bon content, inert fillers, low levels of volatiles or combustible organics, the improved performance and usability of theTGA8000willresultinanenhancedlaboratoryexperience.Thestate-of-theartTGA8000autosamplermakessam-ple handling easier and streamlines labo-ratory procedures, leading to improved laboratory throughput. With the help of TL8000asingleTGAanalysiscancoin-cidewithIRspectroscopy,chromatogra-phy, and mass spectroscopy leading to detailedmaterialscharacterization.Thisadditional information can provide the grist for problem solving and insights leading to product improvement.

References:• IPC-TM-650TESTMETHODSMANUAL,

The Institute for Interconnecting and PackagingElectronicCircuits,2215

SandersRoad,Northbrook,IL60062-6135.

THE BEST ANSWERS HAPPEN WHENGREAT TECHNOLOGIES CONNECT

www.perkinelmer.com/hyphenation

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Global Solutions for Changing WorldWhenregulationskeepchangingandnewenvironmentalthreatsemergeeveryday,onecompanyoffersthetoolsandexpertiseyouneedtorespondquicklyandeffectively:PerkinElmer

Cleaner Water Fresher Air Safer Soil

With most reliable technolo-gies to detect very low con-centration of contaminants indrinkingwater,webringyou the systems with stability tohandlecomplexmatriceswhileachievingrequiredde-tection limits.

Key Applications:•Toxicandtracemetals•Mercurycontent•Mineralcontent•Volatileorganiccompounds(VOC’s)•Semi-volatiles•Greaseandoil•Carbamates•Speciation

Risingairpollutionlevelisposingserioushealthrisksandisnowthearea of top concern all over the world with both developed & developing economiesworkingtowardsreducingcarbon emission and implementing environmental friendly solutions.

We have helped people everywhere breathe little easier with our sophis-ticated air monitoring methods & systems.

Key Applications:•Airtoxics•Airparticulatemonitoring•Ozoneprecursors•Soilvaporintrusion• Industrialhygiene• Incidentmonitoring

For improving soil health and to promotejudicialuseoffertilizers& pesticides, we have solutions forquantifyingmicro-nutrientsand to detect even the smallest concentrationoftoxicmetalsinsoil,solidsandhazardouswastes.

Key Applications:•Toxicandtracemetals•Hexavalentchromium•Mercurycontent•PesticidesandPCB’s•DRO’sandGRO’s•Semivolatilecompounds•Radiationdetection

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Choose the right solution for yourapplication

APPLICATIONS

Metals Pesticides and Residues

Volatiles and Semi-volatiles

Hydrocarbons Radiation

SamplePreparation

AutomatedLiquidHandling

AtomicAbsorption(AA)

GasChromatography(GC)

GasChromatography/MassSpectrometry(GC/MS)

InductivelyCoupledPlasma-MassSpectrometry(ICP-

MS)

InductivelyCoupledPlasma-OpticalEmission

Spectroscopy(ICP-OES)

Infrared(IR)

LiquidChromatography(LC) PAH

LiquidChromatography/InductivelyCoupled

Plasma-MassSpectrometry(LC/ICP-MS)

Speciation

LiquidChromatography/MassSpectrometry(LC/MS)

LiquidScintillation

Thermal Analysis

Ultraviolet(UV/Vis)

Informatics

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COMPLETE SOLUTIONS FOR REFINERY AND NATURAL GAS ANALYSIS

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IntroductionThe drastic increase in production and consumption of engineered nanopar-ticles(ENPs)hasraisedtheconcernandquestionsabouttheirreleaseintothe environment and potential harm toaquaticandterrestrialspecies.Thecharacteristic properties of nanoparti-cles,suchassmallsizeandhighspecificsurfaceareaandreactivity,makethemdesirable for their use in various prod-ucts.

Silver (Ag) nanoparticles are among the most commonly used nanopar-ticles in consumer products due to their antimicrobial properties. There-fore, it is expected that Ag ENPs will find their way into the environment, necessitating a way to accurately and rapidly detect and characterize them in a variety of environmen-tal matrices.Workhasalreadybeenperformed demonstrating the ability to successfullycharacterizeAgENPsinavariety of water samples1-3 and biologi-calmediawhichmaybeexposedtoAgENPsintheenvironment4.

A major source of environmental release iswastewaters,acomplexmatrixwhichmust be evaluated for the fate of Ag ENPs.ThecomplexityandvarietyofthewastewatermatricescanmaketheanalysisofENPschallenging.

Measurement and Analysis of Silver Nanoparticles in Wastewaters with Single Particle ICP-MS

Environment

Authors:Mehrnoosh AzodiSubhasis GhoshalMcGill UniversityMontreal, Canada

Chady StephanPerkinElmer, Inc.Shelton, CT

This work evaluates the ability of SP-ICP-MS to characterize Ag NPs in a dissolved organic solution contain-ing alginate (a common wastewater component) and two wastewater matrices: mixed liquor and effluent.

ExperimentalSamplesandSamplePreparationThewater samples were collected from a wastewater treatment plant near Montreal,Quebec,Canada.Theefflu-ent wastewater was collected after the secondarysettlingtank,whilethemixedliquorwascollectedfromthesecondaryaerationtank.Bothwatertypeswerecollectedinacid-washed,darkglassbot-tlesandsealed.Effluentwastewateristhe ultimate treated wastewater which is discharged to the river from this treat-mentplant,whilethemixedliquoristhewastewater which leaves the aeration tankafterbiologicaltreatmenttothesecondarysettlingtankforthesus-pended solids to sediment. As a result, themixedliquorhasmuchhigherlevelsof suspended solids and relatively higher dissolved carbon content compared to the effluent wastewater.

Alginate is a polysaccharide which is detected in wastewaters at ppm levels and comprises the dissolved organic carbon fraction of wastewaters. The

alginatesolutionwasusedasaknowncontrol/surrogateforcomparisonwiththe wastewater samples. The alginate solutions were prepared from alginic acid sodium salt from brown algae (Sigma-Aldrich,St.Louis,Missouri,USA)at6ppmindeionizedwaterbyshakingend-over-end for an hour.

AgENPscappedwithpolyvinylpyr-rolidone(PVP)withameandiameterof 67.8±7.6 nm (as determined with transmissionelectronmicroscopy[TEM],nanoComposix™Inc.,SanDiego,Califor-nia,USA)werespikedinto10mLofallsamples at a concentration of 10 ppb (5 millionparticles/mL).Thesampleswerethendiluted10-1000xwithdeionizedwater and sonicated for five minutes prior to analysis. All samples were pre-pared in triplicate.

Instrumental ConditionsAllanalyseswerecarriedoutonaPerki-nElmerNexION®300D/350DICP-MSoperatinginSP-ICP-MSmodeusingtheSyngistix™NanoApplicationSoftwareModule.Instrumentalparametersareshown in Table 1. With these param-eters, a transport efficiency of 8.3% was determined.

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Table 1. NexION 300D/350D ICP-MS Instrumental Parameters

Parameter Value

SampleUptakeRate 0.3mL/min

Nebulizer GlassConcentric

SprayChamber GlassCyclonic

RFPower 1600 W

Analyte Ag107

Analysis Time 100 sec

DwellTime 100 µsec

Results and DiscussionTodeterminetheaccuracyofSP-ICP-MS,theAgENPswereaddedtodeion-ized(DI)waterataconcentrationof0.1ppb(50,000particles/mL).SP-ICP-MSmeasurement determined the mean sizeoftheAgENPstobe63.2±0.2nm(whichagreeswiththeTEMmeasure-ments),andtheconcentrationtobe53,758±1363particles/mL,thusvalidat-ing the accuracy of the measurements. The values and standard deviations are from the mean of three replicate analyses.

Next,theAgENPsweremeasuredina 6 ppm alginate solution. Figure 1 showstheAgparticlesizedistribu-tionfor0.1ppb(50,000particles/mL),which corresponds to a mean particle sizeof66.1±0.1nm,withaconcentra-tionof52,302±2102particles/mL.Theagreement between the measured and TEMdeterminedparticlesizesindicatesthatthealginatematrixdoesnotaffectthe measurement accuracy.

Figure 1. Measured Ag particle size distribution in 6 ppm alginate solution.

Figure 2. Measured Ag particle size distribution in ef-fluent wastewater diluted 1000 times.

Withtheaccuracyofthetechniqueestablished in the alginate solution, the effluentwastewaterandmixedliquor

Figure 3. Measured Ag particle size distribution in mixed liquor wastewater diluted 1000 times.

The detection limits for both the Ag particlesizeandconcentrationsinthewastewaters were determined. For the determinationofparticlesizedetectionlimits,thedilutedsampleswereanalyzedwithoutanyAgENPsbeingadded.Thedetection limit was determined by running theunspikedwastewatermatricesandobservingtheparticlesizewhichcorre-spondedtothesmallestpeakrecordedintheSyngistixNanoApplicationModule.For the effluent, the detection limit is about18nm,whileforthemixedliquor,itis about 12 nm.

ThisworkhasdemonstratedtheabilityofSP-ICP-MStoaccuratelydetectandmeasure silver nanoparticles in three different types of wastewater samples. Although wastewater matrices are complex,theydonotinhibittheabilityofSP-ICP-MStoaccuratelymeasurethesizeandnanoparticleconcentration.

Table 2. Results from Analysis of Wastewater Samples Spiked with Ag NPs.

Sample Mean Particle Size (nm)

Spiked Particle Conc. (par-ticles/mL)

Measured Particle Conc. (particles/mL)

EffluentWaste-water

66.3±0.2 50,000 54,691±1185

MixedLiquorWaste-water

63.7±0.4 50,000 53,123±1216

Component Part Number

Green/Orange(0.38mmid)PVCSampleUptakeTubing

N0777110

Gray/Gray(1.30mmid)SantopreneDrainTubing

N0777444

SampleTubes B0193233(15mL)B0193234(50mL)

Consumables Used

samplesweremeasurednext.First,thetotal Ag concentration was measured in both wastewater samples and was found to range from 25-40 ppt, a level which should not inhibit the determina-tionofAgENPs.Figures2and3showthemeasuredparticlesizedistribu-tionsfortheeffluentandmixedliquor,respectively. The samples were diluted 100xpriortoanalysis,withTable2showing both the measured particle sizesandparticleconcentrations.Again,themeanparticlesizeagreeswiththe certificate value, and the particle concentration is close to the calculated value, indicating that neither of the wastewater matrices affects the meas-urement. These results indicate that Ag ENPscanbesuccessfullymeasuredinwastewater samples.

References:• Mitrano,D.,Ranville,J.F.,Stephan,C.,“QuantitativeEvaluationofNanoparticleDissolutionKineticsusingSingleParticleICP-MS:ACaseStudywithSilverNano-particle”,PerkinElmerApplicationNote,2014.

•Hadioui,M.,Wilkinson,K.“AssessingtheFateofSilverNanoparticlesinSurfaceWatersusingSingleParticleICP-MS”,PerkinElmerApplicationNote,2014.

•Dan,Y.,Zhang,W.,Xingmao,M.,Shi,H.,Stephan,C.“GoldNanoparticleUptakebyTomatoPlantsCharacterizedbySingleParticleICP-MS”,PerkinElmerApplicationNote,2015.

•Gray,E.,Higgins,C.P.,Ranville,J.F.“AnalysisofNanoparticlesinBiologicalTissuesusingSP-ICP-MS”,PerkinElmerApplicationNote,2014.

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IntroductionWithwaterqualityvaryingwidelywithgeography and geology, as well as pollution considerations, it is important toknowthemetalcontentofwaters,both for consumption and industrial use. Althoughavarietyoftechniquescanmeasure minerals in water, one of the simplest,leastexpensive,andfastestisflameatomicabsorption(AA)spectrom-etry.Asaresult,thetechniquecontin-ues to enjoy widespread use, despite theincreasingpopularityofICP-OESandICP-MS.

Thisworkfocusesonthedetermina-tionofsevennon-toxicelementsusu-allyfoundindrinkingwaterswiththePerkinElmerPinAAcle™ 500 flame atomic absorption spectrometer. Although other lower-level elements can also be measured by flame AA, these are most commonlyanalyzedbyeithergraphitefurnaceAA,ICP-OES,orICP-MS.

Analysis of Minerals in Drinking Water using PinAAcle 500 Flame AA

Environment

Authors:Deborah BradshawAtomic SpectroscopyTraining and ConsultingKenneth NeubauerPerkinElmer, Inc.

ExperimentalSamplesconsistedofmunicipalandwellwaters collected locally, spring waters purchased from a local grocery store, andacertifieddrinkingwaterstand-ard(TraceMetalsinDrinkingWater–High-PurityStandards™,Charleston,SouthCarolina,USA).Sampleprepara-tion consisted only of acidifying each waterwith1%HNO3(v/v)andadding0.1% lanthanum chloride as a releasing reagentforcalcium(Ca)andmagnesium(Mg)andasanionizationsuppressantforsodium(Na)andpotassium(K).

All analyses were carried out with the PinAAcle 500 flame AA spectrometer using the conditions in Tables 1 and 2.Duetothehighmineralcontent,the burner was rotated 30 degrees to decrease the signal intensity for the analysis of the minerals. In addition, KandNawereanalyzedinemissionmode, which allowed the PinAAcle 500

Table 1. PinAAcle 500 instrument and ana-lytical conditions common to all elements.

Parameter Value

AirFlow(L/min) 2.5

AcetyleneFlow(L/min) 10

ReadTime(sec) 3

Replicates 3

to be auto-configured in such a way to extendtheanalyticalrangesothatevenhigher concentrations could be meas-ured. This allowed minimal dilution for K andeliminationofdilutionforNa.

Sampleswereintroducedviaself-aspi-rationwithahighsensitivitynebulizer,which is standard on the PinAAcle 500 spectrometer.Thenebulizerwasusedwithoutthespacer(providingmaximumsensitivity)forthedeterminationsofcopper(Cu),iron(Fe),andzinc(Zn).Thespacer was inserted for the determina-tionsofNa,K,MgandCa.

“Clean drinking water means be�er health, helps to boost economic growth and contributes to GDP, says PM Narendra Modi during 19th session of Mann Ki Baat programme on All India Radio”.

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Table 2. PinAAcle 500 instrument and analytical conditions specific to each element.

Element Wavelength (nm) Slit (nm) Mode Burner Angle (degrees)

Calibration Standards (mg/L) Calibration Curve

Ca 422.67 0.7 Absorption 30 0.5, 1.0, 2.0, 5.0, 10, 20, 40 Non-LinearthroughZero

Cu 324.75 0.7 Absorption 0 0.05, 0.10, 0.25, 0.50 LinearThroughZero

Fe 248.33 0.2 Absorption 0 0.05, 0.10, 0.25, 0.50, 1.0 LinearThroughZero

Mg 285.21 0.7 Absorption 30 0.5, 1.0, 2.0, 5.0, 10 Non-LinearThroughZero

K 766.49 0.7 Emission 30 2, 5, 10, 20, 30, 40, 50 Non-LinearThroughZero

Na 589.00 0.2 Emission 30 2, 5, 10, 20, 30, 40, 50 Non-LinearThroughZero

Zn 213.86 0.7 Absorption 0 0.05, 0.10, 0.25, 0.50 LinearThroughZero

Results and DiscussionAll calibrations yielded correlation coeffi-cients of 0.999 or greater. The accuracy of the calibrations was assessed with an independentcalibrationverification(ICV)solution, which was diluted 100 times to fall within the range of the calibration curve.TheresultsoftheICVappearinTable 3 and demonstrate the accuracy of the calibration curves.

To validate the methodology, a refer-encematerialwasfirstanalyzed,withthe results shown in Table 4. All recover-ies are within 10% of the certified value, demonstrating the accuracy of the methodology.

Table 3. Results for independent calibration verification (ICV).

Table 4. Results for reference material (all units in mg/L).

Element Concentration (mg/L) Experimental (mg/L) % Recovery

Ca 5.00 4.86 97

Cu 0.25 0.26 104

Fe 1.00 1.00 100

Mg 5.00 4.88 98

K 5.00 4.78 96

Na 5.00 5.12 102

Zn 0.20 0.21 105

Element Concentration (mg/L) Experimental (mg/L) % Recovery

Ca 33.4 35.0 95

Cu 0.022 0.020 110

Fe 0.095 0.100 95

Mg 8.69 9.00 97

K 2.28 2.50 91

Na 5.90 6.0 98

Zn 0.070 0.070 100

Table 5. Results for samples (all units in mg/L).

Element Municipal Water (mg/L) Well Water-1 (mg/L) Well Water-2 (mg/L) Well Water-3 (mg/L) Spring Water-1 (mg/L) Spring Water-2 (mg)

Ca 17.7 0.148 35.3 32.4 3.43 19.2

Cu 0.048 <DL 0.052 0.017 <DL <DL

Fe <DL <DL 0.019 <DL <DL <DL

Mg 6.43 0.026 4.90 5.12 0.799 6.09

K <0 233* 4.89 4.10 0.73 0.69

Na 38.4 3.63 10.9 42.9 6.60 7.25

Zn 0.008 0.043 0.010 0.023 <DL <DL

*Samplerequireda10xdilution

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With the accuracy of the method estab-lished,severaldrinkingwatersamplesfromvarioussourceswereanalyzed.Themunicipal and well water samples were collected directly from a faucet, while the spring water samples were poured from the bottles in which they werepurchased. The results appear in Table 5.ThepresenceofCuandZninthefoursamples collected from the faucet is mostlikelyduetoleachingfromcopperpipes, fittings, and solder. Well Water-1 is interesting as it contains the lowest levelsofallsamples,exceptforanex-traordinarily high level of K. Furtherinvestigation determined that this residence has a water softener installed whichutilizesKasthecounter-iontoremovehighlevelsofCaandMgfromthe well water.

Asexpected,CuandZnarenotde-tected in the spring waters; only the minerals are present. The variation in mineral concentration is indicative of the different geologies of the areas where these waters originate.

Finally, detection limits were determined forCu,Fe,andZnasthreetimesthestandarddeviationoftenblankmeas-urements(i.e.1%HNO3),asshowninTable6.Becauseoftheirelevated

Table 6. Detection limits.

Element Detection Limit (mg/L)

Cu 0.002

Fe 0.006

Zn 0.004

Component Part Number

HighSensitivityNebulizer

N3160144

Autosampler Tubes B0193233(15mL)B0193234(50mL)

CaHollowCathodeLamp

N3050114

CuHollowCathodeLamp

N3050121

FeHollowCathodeLamp

N3050126

MgHollowCathodeLamp

N3050144

ZnHollowCathodeLamp

N3050191

QualityControlStan-dard,21Elements

N9300281

InitialCalibrationVerificationStandard

N9300224

Pure-GradeCaStan-dard(1000mg/L)

N9303763(125mL)N9300108(500mL)

Pure-GradeKStan-dard(1000mg/L)

N9303779(125mL)N9300141(500mL)

Pure-GradeMgStan-dard(1000mg/L)

N9300179(125mL)N9300131(500mL)

Pure-GradeNaStan-dard(1000mg/L)

N9303785(125mL)N9300152(500mL)

ConclusionThis work has demonstrated the ability of the PinAAcle 500 to suc-cessfully measure mineral elements in drinking water samples, including municipal, well, and spring waters. Bytakingadvantageoftheabilitytoro-tate the burner and measure in emission mode, both trace and mineral elements couldbemeasured.WithSyngistixTouch™ software, the PinAAcle 500 AA spectrometercanbeoperatedexclu-sively from a touchscreen interface. For greaterflexibility,theabilitytorunSyng-istix™ for AA software from an on-board computerisalsoavailable.ThisflexibilitymakesthePinAAcle500flameAAspectrometeranexcellentchoicefortheanalysisofdrinkingwaters.

Consumables Usedlevels, detection limits were not deter-minedforthemineralelements(i.e.Ca,K,Mg,Na).Inaddition,sincetheseele-ments are usually present at high con-centrations, the instrument was detuned for their analysis. Therefore, detection limits would be meaningless.

Fully contained maintenance-free fiber optic technology in PinAAcle AA spectrometers, enhances light throughput for best detection limits.

PinAAcle™ 500 Flame AA

Experience the new PinAAcle of performance in Flame AA

Engineeredtodeliveranuncompromisinglevelofperformanceatanunbeatable price, the PinAAcle 500 puts the industry’s most robust, reliable Flame AA within reach of even the most budget-conscious laboratories.

• Offerssuperiordurability,longerlife,lowermaintenancecostsandfast-estROIofanyFlameAA.

• Real-time,truedouble-beamoptics.• Exceptionalsensitivityandprecision(Achieveprecisionoflessthan0.3%).

• Completelycorrosion-resistantdesign(Conformal-coatedcircuitboards),handles harshest environments and corrosive samples.

• Fast,simple,reproducibleoperationwithquickchange,modularsampleintroduction system.

• Compatibilitywithsampleautomationplatforms–FASTFlame,AutoPrep50andS10autosampler.

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IntroductionAqualitativerapidandreliablemethodfordetectionofPolyvinylChloride(PVC)indifferentpackagingmaterialscanbe achieved by a simple ielstein Test followedbyFT-IRmeasurement.Themethod involves spotting characteristic absorptionbandsofPVCinthesam-plebycomparingitwithstandardPVCspectra.

PolyVinylChloride(PVC)isoneofthe most important and widely used thermoplastics due to good process-ability, chemical resistance, and low lammability. The physical property of PVCcanbecontrolledbyvaryingtheplasticizercontent.PVCsareusuallyusedaspackagingmaterials,wires,films and sheet, floor tiles, and a variety ofsoftchildren’sproducts.Duetothepersistent, bio-accumulative nature of manyofthechemicalsreleasedbyPVCproduction, their effects are irreversible andposeahugeenvironmentalrisk.Textileindustrycompliancerequiresthatmaterials, chemicals, parts, and other goods, used or supplied in the manufac-tureoftextileproducts,complywiththeapplicable chemical content and chemi-calexposurelawsofeverygovernmentaljurisdiction in which those products are

Rapid and Reliable PVC Screening in Packaging Material used in Textile Industry

Textile

manufactured or distributed to protect the health and safety of consumers and others handling finished products. TheRSL(RestrictedSubstanceList)offinished products, including apparel, non-apparel, footwear, accessories, and otherproductsrequiresthatparts,othergoods, and finished products provided by suppliers and sources comply with the“LimitValueFinalroduct”(LVFP)levels.TheuseofPVCinthepackagingmaterialinthetextileIndustrycomesunderRSLandthereisacompletebanontheusageofPVC.ThemandatoryrequirementforscreeningthismaterialhastobetestedusingtheBeilsteintestandFT-IRforconfirmation.

ExperimentalIn this application note we show that BeilsteinandFT-IRtestingcanbeusedtoconfirmthepresenceofPVCinpackag-ingmaterials.Herewehaveusedvariouspackagingplasticsastestsamples.ThepresenceofhalogensusingtheBeilsteintest in any material containing bound or ionic halogens (chlorine, bromine, iodine)suchassaltorpolyvinylchloride(PVC)willreactwithacopperwirewhenheated in a flame and produce a bril-liant, long-lasting green flame indicating the presence of halogens. The pres-

ence of a greenish flame indicates the presence of halides. The flame will burn greenforalongperiodoftimeifPVCsarepresent.ForPVCconfirmatorypres-ence,FT-IRmeasurementwascarriedoutonaSpectrumTwo™FT-IRusingaDiamondATR.Experimentalparametersused for measurement were scanning range of 4000 – 400 cm-1, resolution of 4 cm-1 and 16 scans.

Table 1. Characteristic IR spectra absorption bands for PVC.

Spectral Range (cm -1) Functional Assignment

2900 to 3000 AliphaticC-HStretch-ing

1725 to 1740 EsterPeakforPhthal-atesplatsticizers

Peakaround1426 BendingofaliphaticC-HBonds

Peakaround1240to 1260

BendingofC-HbondsnearCl

Peakaround1000 StretchofC-Cbonds

Doubletat610and630andpeakat695

C-Clgauchebond

Authors:Sushant JadavDr. Manohar RaoPerkinElmer, Inc.India

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Data AnalysisThe following samples were tested by PerkinElmerSpectrumTwoinstrumentwithDiamondATRforPVCqualifica-tion.SamplesspectralistedinFigure2

weremonitoredforPVCcharacteristicabsorptionbands.GiveninFigure2arethe spectra of each sample with obser-vations.

Figure 2. The IR absorption spectra show the confirma-tion of PVC in Sample 1 and Sample 2, while the absence of PVC in Sample 3.

Figure 1. Spectrum Two with Diamond ATR .

ConclusionInordertocharacterizeandidentifythepresenceofPVCinplastics,aBeilstientestfollowedbyFT-IRanalysiswascarriedout.ForPVCwhichisbannedinpackagingmaterialinthetextileindustry,FT-IRwithATRtechniquecanbe used as a verification test which is a very fast, reliable, cost effective method forPVCqualificationwithagooddetec-tion limit. The methodology provides theabilitytoscreenPVCqualificationofdifferent samples with little or no sam-ple preparation. The portability of the PerkinElmerFT-IRsystemenablesthesemeasurements to be made in the field and help to ensure that plastic parts and objects do not enter the commercial marketplace.

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Azodyesarecompoundscharacterizedbytheirexcellentcoloringproperties.They are important and widely used as coloringagentsinthetextileandleatherindustries.Theriskintheuseofazodyesarisesmainlyfromthebreakdownproducts that can be created in vivo by reductivecleavageoftheazogroupintoaromaticamines.Duetothetoxicity,carcinogenicity and potential mutagenic-ity of thus formed aromatic amines, the useofcertainazodyesastextileandleathercolorants,andtheexposureofconsumersusingthetextileandleathercoloredwithazocompoundscausesaserious health concern.

Thetwomainroutesofconsumerexpo-surearetheskinabsorptionoftheazocompounds from the dyed clothes worn, and potential oral ingestion, mainly referringtothesuckingoftextilesbybabiesandyoungchildren.TheEUCom-mission classified 22 amines as proven or suspected human carcinogens & limits their concentrations up to 30 ppm.

Azo-dyes analysis by GCMS (DIN EN 14362-1: 2012-04) TheENISO17234-1standardmethodfortheanalysisoftextilesmadeofcellu-loseandproteinfibers,forexamplecot-ton,viscose,wool,orsilkisthechemicalreductionofazodyesfollowedbysolidphaseextraction(SPE).

Analysis of Azo-Dyes, Chlorinated Phenols, Organotin and PAH’s in textiles

Textile

Authors:Bruce CasselSaurabh PatelPerkinElmer, Inc.Shelton, CT

ForallthesaidAzodyestheDINEN14362-1:2012-04methodisusedwhichrecommendsanalysisusingGCMSsystem.PerkinElmerClarusSQ8GCMSismostsuitableandflexiblesystemtoprovide very reliable analysis as per the global norms.

Chlorinated phenols in textiles (DIN EN ISO 17070:2007)To prevent mold spots caused by fungi, chlorinatedphenolslikePCPareapplieddirectlyontextiles,leatherandwood.PCPisverytoxicandregardedasacancer-inducingagent.SoitisimportanttodeterminetheexactquantityofPCPintextiletoavoiditscarcinogeniceffecton human health. These compounds are determinedbyClarusx80Gaschroma-tographwithElectronCapturedDetec-tor(ECD)orClarusSQGCMSalsocanbe used for better identification. In most of the cases compounds are monitored aspertheDINENISO17070:2007method.

Analysis of Organotin compounds in textiles by GCMS (BS ISO 17353:2004 (German Version: DIN EN ISO 17353:2005)SyntheticfibresinparticularwerefrequentlytreatedwithTBT,monobutyl-and dibutyltin. The organotin com-pounds prevent the development of an

unpleasantsmellintextilesduringheavysweating. All organotin compounds areconsideredtobetoxic.Themostnotoriouscompoundistributyltin(TBT),averypersistentandhighlytoxiccellpoisonthatisdifficulttodegrade.TBTis one of the most poisonous com-pounds released into the environment, and in humans it causes damage to the hormonal, immune and central nerv-ous systems as well as to the liver and kidneys.ThepermissibleconcentrationofTBTvalueof0.025mg/kgtextile,andfor other organotin compounds a value of0.25mg/kg.

Polycyclic-aromatic Hydrocarbons Content (PAH) in textiles by GCMS (ZEK-01.4-08)PAH’sarewidelyusedinvarioustextileproducts. These are mostly carcinogenic innature.Somearegenotoxictoo.e.g-benzopyrene.Hencerecently,theGermanBoardforTechnicalWorkEquipmentandConsumerProducts(AtAV)hasfurtherextendedthelistofmandatoryPAHs(16byEPA)to18PAHsfortheGS-certificationprocess.Allthesecanbeanalyzedeasilywithbestdetec-tionlevelswithPerkinElmerClarusSQ8GCMSsystem.

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Textileiscategorizedaccordingtoitsutilizationintoproductsforbabies,productswithdirectcontacttoskin,productswithoutdirectcontacttoskin,anddecorativematerials.Forriskestima-tionsthedeterminationoftheextract-able amounts of heavy metals is of importance, due to possible impact on human health. According to the recently introduced regulation, common heavy metalsextractablewithsyntheticgastricjuicefromtextileusedinbabyclothesand toys should also be monitored. This method simulates contact with gastric juice when a material has been swal-lowed.

Toxic effects of textile dyesToxiceffectsofheavymetalsonhumanhealthareverywellknown:damagesof organs, disorders in the respiratory tract and lung diseases, dysfunction of the heart, blood and blood producing organs,skindiseasesandsomeothers.Duetothetoxicityofsomeheavymet-als, guidelines for testing of these metals intextileproductshavebeenprovidedvideISO105E04methodology.

Themajorchemicalpollutantsontextilesare dyes containing carcinogenic amines andtoxicheavymetals.Heavymetalscanexistinnaturalstructuresoftextiles

Determination of Extractable Metals in Textiles as per ISO 105 E-04 Methodology

Textile

Authors:Bruce CasselSaurabh PatelPerkinElmer, Inc.Shelton, CT

ortheycanpenetrateintotextilesduringtheir production, dying process or via the protection agents used for the stor-age or from the environment.

PerkinElmer analyzer for ISO 105 E04 methodTheextractablemetalsfoundinthegarments and fabric may vary in their concentrations from product to product. HenceitisnecessarytohaveasystemlikeNexION350;wheretheultra-tracemetals in a wide range of sample types can be measured.

The common heavy metals can be easily digestedusingTitanMPSmicrowavedigestionsystem.Howeverforthedeterminationofextractablecadmium,chromium,copper,leadandnickelintextilesasperthepublishedmethodtheextractionprocedurerecommendsTex-tileTestingISO105E04Methodologysyntheticgastricjuiceasanextractant.Thisprocessisrequiredtobeoptimizedfor consistent results.

A complete analyzer with support•PerkinElmerISO105E04analyzersystemissuppliedwiththeNexION350ICPMSorOptima8x00ICPwithrequiredsoftwareforcontrolanddataacquisition.

•ItisrecommendedtohaveTitanMPSfor the digestion process.

•Pre-installationandsitereadinessguidance

•Extensiveoperatorstrainingandap-plication support

•Readytousemethodsashandholdingapproach.

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Permissible limits of the extractable metals in textile (non- metallic parts) ISO 105 –E04 (2013)

Extractable heavy metals

Limits mg/Kg

Arsenic(As) 0.2 Usagebannedas biocide

Antimony(Sb) 5 Usageasflameretardant

Lead(Pb) Traces 0.2

Usagebanned

Cadmium(Cd) Traces 0.1

Usagebanned

Mercury(Hg) Traces:0.02

Usagebanned

Copper(Cu) 25-50 Complexdyedtextiles

Chromium(Cr) 0.5 to 1.0 For metal dyed complex

ChromiumVI(CrVI)

<0.5 Usagebanned

Cobalt(Co) 1.0-4.0 For metal dyed complex

Nickel(Ni) 1.0-4.0 Complexdyedtextiles

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IntroductionWith revision to General Notices 5.60.30 Elemental Impurities in USP Drug Products and Dietary Supple-ments, January 1, 2018 is the date on which General Chapters <232> and <2232> will become broadly appli-cable to drug products (<232>) and finished dietary supplement dosage forms (<2232>) in the USP-NF. The removalofreferencesto<231>fromUSP-NFmonographsalsowillbeofficialasofJanuary1,2018.

Thesenewmandateswillsoonrequirea more demanding elemental impurities method to be in place – and in opera-tion–withinyourorganization.

USP’sChapter232(ElementalImpurities-Limits)specifiesthelistofelementsof

Implementation of USP Chapters <232><233> using NexION 350 ICPMS and ICH Q3D Toolkit

Pharmaceuticals

Authors:Mehrnoosh AzodiSubhasis GhoshalMcGill UniversityMontreal, CanadaChady StephanPerkinElmer, Inc.Shelton, CT

concern, potentially found as contami-nants in pharmaceutical products and theirmaximumdailydosebyelementand delivery mechanism (oral, par-enteral, large-volume parenteral, or inhalation).Chapter233(ElementalImpurities-Procedures)detailsthesamplepreparation, analytical procedures, and qualitycontrolvalidationprotocolsthatarerequiredformeasuringtheelementsspecifiedinChapter232.

TheInternationalConferenceonHarmo-nisationofTechnicalRequirementsforRegistrationofPharmaceuticalProductsforHumanUse(ICH)isworkingtohar-monizethemajorglobalpharmacopeias’approach to heavy metal testing, to provide a global policy for limiting metal impuritiesqualitativelyandquantitativelyindrugproductsandingredients(ICH

Q3D–GuidelineforElementalImpuri-ties),specifying24elementalimpuritiesincluding15outlinedinUSP<232>.

PerkinElmer offers a complete, integrated solution to USP 232/233 compliance, including:

•Fast,safeandcost-effectivesam-plepreparationequipment

• Intelligentsamplehandlingthatincludes automated auto-dilution systemsforUSP233methods

•Choiceofbest-in-classICP-MS/ICP-OESandsoftwaresolutions

•Completevalidationservices,•EnhancedSecurity™ software to helpcomplywithRegulation21CFRPart11

USP Chapter <232> key points summarized

•Chapter<232>-specifiesthelistofelementsandtheirtoxicitylimits(maximumdailydosesofdifferentdrugcategories)as:

-Maximumpermissibledailyexposure(PDE)values(referTable1) -Modeofadministration:Oral,Parenteral(intravenousinjection),Inhalation andLVP

•FollowingonfromICHQ3DStep4inDec2014,thelimitsinChapter<232>havebeenupdatedtoalignwithICHQ3D.

•December1,2015:UpdatedchapterhasalreadyappearedinsecondsupplementtoUSP38-NF33withmodifiedlimitsasproposedinICHQ3D.

Thetoxicityofanelementalimpurityisrelatedtoitsextentofexposure(bioavailability).

Exposurefactorisusedtomodifythepermissibledailyexposures(PDE’s)onthe route of administration, assuming 100% bioavailability for parenteral and inhalationroutes.(refer:TargetValuecalculatoronpageno.23)

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USP <233> specifies 4 different sample preparation techniques:

Preparing insoluble samples as per USP <233> guideline using Titan MPS™ Micro-wave Digestion System

Implementing analytical procedures 1 and 2 as described in Chapter <233>

•Useneat,undilutedsample,ifinsuit-ableliquidform

•Diluteinaqueoussolution,ifsolublein water

• Ifnotsolubleinwater,diluteinap-propriate organic solvent

Forinsolublesamplesthatrequireclosed-vessel acid digestion, our Titan MPS™ system is the ideal solution. This top-loading microwave employs a triple-interlockedlidthatallowseasyloading

With the lowest detection limits of any ICP-OESandafullsuiteofenhanceddatasecurityfeatures,PerkinElmer’sOptima®8x00seriesICP-OESmakesiteasy to comply with stringent regula-toryrequirements.DualviewingoftheplasmaallowstheOptima8x00ICP-OESto provide a wide calibration range for enhanced productivity. Added features, such as superior interference correction and patented Flat Plate™ plasma tech-nologymaketheOptima8x00ICP-OESeasy to use and easy to maintain.

The bottom line is that depending on the element and the mode of adminis-

ThereisnoquestionthatICP-MSisthemostsuitablemulti-elementtechniquefor determining elemental impurities at levelsspecifiedinChapter<232>forpharmaceutical products. The desired limits, even for the large volume paren-terals(LVP)atamaximum2Ldosagelevel, which are the lowest specifications of all the different drug delivery meth-ods, can be reached with relative ease.

PerkinElmer’sNexION350ICPMSwithpatentedUniversalCellTechnology™ (UCT)offersthesimplicityofbothcolli-sioncellandexceptionaldetectionlimitsof true reaction cell.

Chapter <233> describes two analytical procedures with associated sample preparation steps for determi-nation of elemental impurities in the drug products, Procedure 1: ICP-AES/OES and Procedure 2: ICP-MS

Table 1. Modified maximum permissible daily exposure (PDE) values (in µg/day) for the administration of drug prod-ucts, based on an “average” 50 Kg person

Including elements specified in ICH Q3D guidelines:

Elements USP <232> Class Oral Daily Dose PDE* Parental Daily Dose PDE (ug/day) Inhalational Daily Dose PDE (ug/day)Cd Yes 1 5 2 2Pb Yes 1 5 5 5Asb Yes 1 15 15 2Hgb Yes 1 30 3 1Co No 2A 50 5 3V Yes 2A 100 10 1Ni Yes 2A 200 20 5Ti No 2B 8 8 8Au No 2B 100 100 1Pd Yes 2B 100 10 1Ir Yes 2B 100 10 1Os Yes 2B 100 10 1Rh Yes 2B 100 10 1Ru Yes 2B 100 10 1Se No 2B 150 80 130Ag NO 2B 150 10 7Pt Yes 2B 100 10 1Li No 3 550 250 25Sb Yes 3 1200 90 20Ba No 3 1400 700 300Mo Yes 3 3000 1500 10Cu Yes 3 3000 300 30Sn No 3 6000 600 60Cr Yes 3 11000 1100 3

a PDE = Permissible daily exposure based on a 50 kg person b See Speciation Section of USP <232>

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VOLUME 49 • Summer Edition, 2016

USP <232>/<233> and ICH Q3D ToolkitTheUSP<232>/<233>andICHQ3Dguidelinesoffergreatbenefits to consumers, but also provide some challenges for pharmaceuticalmanufacturers.WiththenewUSP/ICHToolkit,you can rest assured that complying with these limits and proce-dureswillbeeasierthanever.TheToolkitprovides:

•Informationtohelpgetyoustarted•Toolstoassistwithstandardpreparationandmethod

development•Methodvalidationreportingtool•StandardOperatingProcedures(SOP)•Samplepreparationmethods•NexION® software information

TheUSP/ICHToolkitincludesaJValueCalculatorforaccuratecalculationsofTargetLimits(Jvalues)ofelementalimpurities,makingstandardpreparationandmethoddevelopmenteasier.TheToolkitalsohelpsimproveefficiencieswiththeMethodValidationReportTool,whichcalculatesandsummarizesmethodvalidation data instantly.

With this one tool you’ll be complying with the elemental impu-ritiestestingrequirementsinnotime.

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Download the white paper detailing the elemental & dosage form specific PDE values and analytical procedures as specified in USP Chapter <232> <233> and ICH Q3D guidelines Click here

References:• http://www.usp.org/sites/default/files/usp_pdf/EN/faq/ei-implementation-faq-2015-03-27.pdf• http://www.ich.org/products/guidelines/quality/article/quality-guidelines.html

and removal of vessels, while the poly-mer-coated, stainless steel construction providesmaximumcorrosionresistance.

tering the drug, careful evaluation of the ICP-AES/OEStechniqueisneededbeforeselecting it for this analytical procedure.

With its patented ion optics design (Tri-pleConeInterfaceandQuadrupoleIonDeflector),nomatrixparticulateentersthe mass spectrometer, thereby dramati-cally reducing routine maintenance.

Calculate target limits (acceptance value of the elemental impurity being evaluated) using unique J value calculator:

J Value (Target Limit) is calculated by:

PDE

(MaximumDailyDose×DilutionFactor)

For example: Hg has an Oral Daily Dose PDE of 15 µg/day. If we digest 0.1g of a material that has a daily dosage of 1 g and dilute the resulting solution to 50 mL, the J value with therefore be:

15µg/day

1gX0.1g day50mL

J=

J=

=30µg/L

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Implement USP <857> Compliance with Lambda 365 UV-Vis Spectrophotometer

Pharmaceuticals

UntilthisyeartherelevantchaptersinUSPharmacopoeiaforUV-Visspec-trophotometrywereGeneralChapter<851>Spectrophotometry&LightScatteringandGeneralChapter<1058>AnalyticalInstrumentsQualifications.AspartoftheUSP–NFmodernisationprocess,theGeneralChapters(Chemi-calAnalysis)ExpertCommitteehasreviewed chapters holistically to align concepts and contents to ensure consist-ency,resultinginsuiteoftechniquespe-cificGeneralChapters-UltravioletVisibleSpectroscopyChapterUSP<857>.Thischapterdetailsqualificationsregardingthe parameters of wavelength accuracy, photometricaccuracy/linearity,straylight, and resolution that must be met onaUV-Visiblespectrophotometer.

WiththisinstrumentvendorIQ/OQ,PQ,IPVdocumentsandsoftware,previousqualificationorcalibrationSOPsandworksheetsarenowout-of-date.

USPharmacopoeiaGeneralChapterUSP<857>isnowofficialinNF38;howeverit is staged to become mandatory in USPNF39from1stMay2016.Hence,allFDAauditorsvisitingpharmaceuti-callaboratorieswillbenowrequiredtoidentify instruments & labs globally that needtocomplyfor:

•Testingdrugorintermediateorexcipi-entthatissoldinUSA

•MethoddevelopmentlabsfordrugorintermediateorexcipienttestingsoldinUSA

•Labswherefulllatestinternationalcomplianceisrequiredbyinternalpolicyorcustomerexpectations

Knowing the upgrade route to re-main compliantPerkinElmerhasthoroughlyinterpretedtherequirementsofUSP<857>asNewChaptersinUnitedStatesPharmacopeiawill affect compliance status now. This leavesexistingdoublebeamUV-VisspectrometersandDiodeArrayspec-trometer of most of the international brandscertifiedwithvendorIQ/OQ/PQ,IPVdocumentsandinstrumentsoftwareoutofdate.TheestablishedSOPsforcalibration of the instruments will not hold good.

TheUSP<857>effectivelyextendsthetesttoUVandVisiblerange.TheEPlimitsthetesttoUVregion.PerkinElmerLambda25,35and45(notolderthan5years)areguaranteedtopassallUSPandEPrequirements.PerkinElmeroffersUOQasserviceandrecordofcompli-ance including the new stray light procedure.

New Lambda 365 UV-Vis spec-trometer with UOQ

For all laboratories under regulatory environment; it is worth having the con-siderationforlatestLambda365UV-Visspectrometerwithstate-of-the-artUV/Visperformancethatmeetstheneedsof pharmaceuticals, analytic chemists, geneticists,andmanufacturingQA/QCanalysts. It has following salient features whichsuittheUSP<857>criteria:•Wavelengthrange190to1100nmwithaccuracyof+/-0.1nm

•Truedoublebeamsealedopticswithlow stray light

•Variableslitwidth0.5,1,2,5,20nm•DualSiliconphotodiodesandwider

dynamic range up to 4 Abs•Wavelengthscan,scanningkinetics,bio-applications,quantificationetc.standard functions

•Widerangeofaccessoriesforsolidandliquidsamplesandremotemeas-urement capability

•FullycontrolledbyPCwithWindows’7 or 8 environments

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VOLUME 49 • Summer Edition, 2016

PerkinElmer UOQ offering

•TheUOQforUVProtocolandQualificationReportirrespectiveofmanufac-turer

•AllofthetestproceduresandformuladescriptionsareembeddedintheProtocol

•Anautomated,fully-configurable,fastandsecuremethodtoqualifyinstru-mentsutilizingyourexistingdataacquisition

•Easyreviewandautomatedcalculationsaswellaspass/faildetermination•UOQforUVcanbedeliveredonanystandardUV-VisSpectrophotometermadebyPerkinElmerorothermanufacturers

•UltrasecuresmartPDFreportformatwithuniqueIDanddigitalcertificate•UOQforUVmeetsUSP<857>,EPandJPregulations

For further information and upgrade of

yourexistingLambdaUV-Visspectropho-

tometerforUSP<857>,requestcontact

CONSUMABLES FOR

SEAMLESS CHROMATOGRAPHY

APPLICATIONS

AtPerkinElmer,we’recommittedtoprovidingyouwiththebestselectionofsolutionsforallyourChromatogra-phyneeds,regardlessofmake,modelormanufacturer.We have invested heavily in growing our portfolio, at your request,tobringthebestperformingandproductivityenhancing consumables and accessories for all your gas chromatography systems. Requestforyoure-copyofconsumablescatalogClickhere

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ts• Finestquality,high-strengthfusedsilicacapillarycolumns(bothgeneralpurposeandspecialtyphases)-Eliteseries.

• BrownleeSuperficiallyPorousParticle(SPP)columnsforgreaterspeed,lastingdurabilityandbetterresultsfromLCinstrument.

• Highestqualitygaschromatographconsumables-Vials,caps&septa, liners, ferrules & connectors, autosampler syringes, nuts, organic standards etc. to fulfill all laboratory needs.

• Highqualitygasfilterationsystems.• FlowMarkelectronicflowmetersprovidecontinuousreal-timemeasurementsofgasstreamsflowrangingfrom0.50mL/minto500mL/min.

• Compacthandheldelectronicgasleakdetectoristheidealsolutionfordetectinggasleaksinyourgaschromatographysystems.

References

http://www.usp.org/usp-nf/development-

process/publication-comment-schedule

Choose from one of the widest selections of GC, GC/MS, LC and LC/MS Columns, Vials, Septa, Caps and more:

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VOLUME 49 • Summer Edition, 2016

Determination of CholesterolLevel in Human Serum -Enzymatic Colorimetric Method

Pharmaceuticals

IntroductionClinicalchemistryuseschemicalpro-cesses to measure levels of chemical components in the blood. It is very useful for the early diagnostic of disease and for monitoring organ function. The most common specimens used in clinicalchemistry are blood and urine. Table 1 shows the common blood tests and measurableitemsusingUV/Visspectro-photometers. In this application note, the cholesterol level in human serum wasdeterminedbytheenzymaticmethodusingtheLAMBDA™465UV/VisSpectrophotometerandUVLab™ software.

PrincipleThe cholesterol esters of the sample arehydrolyzedbycholesterolesterase.4-Cholesten-3-oneandH2O2 are then formed from the released free cholester-olbycholesteroloxidase.Ameasurableredquinoneiminederivative,thathasanabsorbance at 500 nm, is formed from hydrogenperoxide(H2O2)and4-amino-antipyrine in the presence of phenol and peroxidase.

Reagents and Apparatus1.Cholesterolbuffersolution(Choles-terolkit,100mL)-phenol132mg,NaH2PO40.78g,NaH2PO40.71g

2.Enzymereagent(Cholesterolkit,100mLdilution)-cholesteroloxidase12unit, cholesterol esterase 3.5 unit,

peroxidase6700unit,4-aminoantipy-rine17.0mg/dL

3.Cholesterolstandardsolution(Choles-terolkit)-300mg/dL

4.Humanserumsample5.D.Iwater6. Water bath7.LAMBDA465(UV/VisSpectrophotom-eter)

8.UVLabsoftware9.Cuvettes(10mmpathlength)

Procedure1.Prepareanenzymesolutionbydissolv-ingtheenzymereagentto100mLinthe cholesterol buffer solution.

2.PreparethemixtureasshowninTable2.3.Placeinawaterbathat37°Cforfive

minutes.4.Measureblanksolution.5.Measurestandardsolution.6.Measuresamplesolution. (Performthemeasurementquickly,withinonehour).

Cholesterollevelsinserumarecalcu-latedusingEquation1.(Normalrange:130-250mg/dL)

A schematic representation of the reac-tionisshowninEquation2.

Equation 1

Cholesterol=Level(mg/dl)

Absorbance ofSample

X300···(1)Absorbance ofStandard

Equation 2

Cholesterolester

Cholesterolesterase

Cholesterol+

fatty acids

Cholesterol

Cholesteroloxidase

Cholest-4-en-3-one+

H2O2

2H2O2+Phenol+4-Aminoan-tipyrine

Peroxidase Quinonei-mine+

4H2O

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Table 1. Common blood tests and measurable parameters using UV/Vis spectrophotometer.

Table 2. Mixture preparation for measurement.

Table 3. Cholesterol level in human serum.

Common Blood Tests Tests using UV-Vis Spectrophotometer

WBC,RBC,Hb,HCT,MCV,MCH,MCHC,Platelet,GOT,SGPT,ALP,y-GTP,Totalprotein,Albumin,Totalbilirubin,BUN,Creatinine,Uricacid,Totalcholesterol,Triglyceride,LDH,CPK,Amylase,Glucose,VDRL,anti-HIV,HBsAg,HBsAb,Fe,P,Ca,Mg

Hb,SGOT,SGPT,ALP,y-GTP,Totalprotein,Albumin,Totalbilirubin,Creatinine,Uricacid,Totalcholesterol,Triglyceride,LDH,Amylase,Glucose,Fe,P,Ca,Mg

Common Blood Tests Blank Standard Sample

Enzymesol. 3 3 3

D.IWater 0.02

Cholesterolstd. 0.02

SerumSample 0.02

Name AU(500 nm) Concentration (mg/dL)

Standard 0.2775 300

SerumSample 0.2348 253.84

Instrument ParametersTheLAMBDA465instrumentparam-eters are as follows. Figure 1 shows experimentalmethod.

Experiment SetupDatatype:AbsorbanceSampling:SinglecellMode:Scanno.:30;Integrationno.:1

Figure 1. Experimental method.

ResultFigure 2 shows the spectra of cholester-ol. The absorbance values and choles-terol level of serum sample are shown in Table 3. The determined cholesterol level inserumis253.84mg/dLcalculatedusingEquation1.

Figure 2. Absorption spectra of cholesterol by enzy-matic colorimetric method.

ConclusionThe determination of cholesterol level in humanserumbyenzymaticcolorimet-ric method was performed using the LAMBDA465UV/VisspectrophotometerandtheUVLabsoftware.Afterthe

reaction, the measurement time was minimizedusingtheLAMBDA465,ena-blingustocollectdataquicklyoverthefull wavelength range from 190 to 1100 nm.Dataprocessingwasperformedef-fectively by the powerful and easy to use

software. The calculated cholesterollevelbyEquation1wasslightlyhigherthanthenormalexpectedrange(130-250mg/dL).

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•AutomatedEight-CellChanger•AdvancedTransmissionSampleHolder•Six-CellPeltierHolder• IntegratingSphere•FixedAngleReflectanceAccessory•VariableAngleTransmissionAccessory•MicrosamplingCell•VariablePathlengthCuvetteHolder•FiberCouplingModule

*This application note is for research purpose only.

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VOLUME 49 • Summer Edition, 2016

Expanding Food Testing Capabilities further with Perten Instruments

Food Testing

We are very pleased to announce that PerkinElmerInc.hasenteredintodefini-tiveagreementtoacquirePertenInstru-mentsGroupAB,basedinStockholm,Sweden.ByaddingPerten’sanalysisplatforms, along with its leading food qualitycalibrationdatabasetotheexist-ing portfolio of analytical instruments, wearenowholisticallyequippedtofirmly assist our customers in address-ingrigorousregulationsforfoodqualitycontrol,import/exportproducttestingand the need to preserve the integrity of global supply chains.

Perten is a leading global supplier of ad-vancedanalyticalinstrumentsforqualityof food, grain, flour and feed. Typical offeringsinclude:

1.NIRAnalyzers(Lab,On-lineandIn-line)

2.FallingNumberSystem3.LabMills4.TextureAnalyzer5.GlutomaticSystem6.FoodViscosityAnalyzer

ThenewDA7250NIRanalyzeristhethirdgenerationdiodearrayNIRinstru-ment from Perten, designed specifically for analysis in the food and agri indus-tries.TheDA7250comespre-calibrat-ed for a wide range of applications, anddeterminesfollowing:

Parameters:Moisture/DryMatter,Protein,Fat/Oil,Ash,Fiber,Starch,AminoAcids,FattyAcids,Sugars,Brix,Lactose,andmore.

Samples:Grains,Pellets,Powders,Pastes,Slurries,Liquidsandmore,theDA7250excelsindusty,dirtyandoth-erwise challenging environments.

•Minimalornosamplepreparation•Nomovingopticalcomponents•RapidandNon-Contactanalysisin

seconds•Factorycalibrationsavailableforwide

range of applications•Globaldatabaseofmorethan

100,000 samples• IP65certifiedfordustandwater

resistance•Lab,In-LineandAt-Lineversions

Inexpensive sample modules with quick changeover and minimal clean-up.

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www.perten.com

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Asia Pharma Expo and DTG-2016, Dhaka, Bangladesh | 28-31st Jan, 2016This year we participated in Asia Pharma ExpoandTextile&GarmentMachineryExhibitiontoconnectwithprofessionalsfrompharmaceuticalandtextileindustry, which are priority sectors in Bangladeshwithtextilecontributingto80%ofexportsearningsandpharmaindustry gearing up for investments in their manufacturing and testing infrastructureforexploringregulatedmarkets.

IAIA - Anacon Seminar Series, Vapi, Gujarat | Environmental Monitoring and Analysis | 27th Feb, 2016Thiswasthe1stofplannedseminarfromseriesandthetopicwasmuchsuitedtocurrentissuesforVapiindustrialareawherechemicalindustriesarethemaincauseofpollution.Eminentspeakersfromvariousindustriesandorganizationspresentedtheconcernsandsolutionsrelatedtoenvironment.WediscussedsolutionsformonitoringRoHStoalltheindustriesandourdaytodayappliancesdisposalwithemphasisonuniquespeciationcapabilities.

ICEFN-16, Kumaun University, Nainital and ICNANO-2016 @ VTU, BangaloreWe sponsored two international conferencesonNanotechnologywhichis widely discussed due to its range of applications, but as with any new technology, nanotechnology has also raisedmanyconcernsabouttoxicityandenvironmental impact of nanomaterials. Our focus was on application capabilities ofSP-ICPMS,toidentifyandmeasurenano-particles(ENP’s,Ag,TiO2etc.)in waste water, cosmetics, dietary supplements etc.

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NCL, Pune Service and PU, Chandigarh UV Vis and FTIR Workshop | April, 2016Recently,weorganizedservicecampinNationalChemicalLaboratory,Puneforinstrumenthealthcheckup,todiscusstheconcernsandrecommendpreventivesteps to end-users for instrument maintenance. Team also suggested suitable consumablesandimportanceofAMC/CMCforlongerinstrumentlifeandminimaldowntime.

SophisticatedAnalyticalInstrumentationFacility(SAIF),PanjabUniversity,conductedaweeklongworkshoponspectroscopytechniquesparticipatedby70facultymembersandSRF’sfromPU,SLIET,IACSetc.SincewehaveUVVis-Lambda750andFTIR+FIR-Spectrum400installedinPU,sowesupportedthemwithtwodayshandsonapplicationandtroubleshootingtrainingsession,executedbyPratikDeshmukhandAmarinderSinghwithSalesandMarketingsupport.

Enhancing Analytical Capabilities Seminar, Visakhapatnam | 29th April, 2016Lastyearwestartedwith“EnhancingAnalyticalCapabilities”seminarserieswithanobjectiveof:•Updatingourcustomerswith

instrumentation and application capabilitiesofexistinganalyticaltechniquesandnewtechnologicaladvancements for enhanced applications, through 30-35 minpresentationeachonkeytechnologies.

•Togiveanoverviewonaddressingregulatorychallengesusingexistingandadvancedanalyticaltechniques

Continuingwithsamethisyear,seminarwasconductedinVisakhapatnamon29thApril,2016eveningatHotelFortuneInnSreeKanya.Wehadaround130attendeesfrompharmaceuticalorganizationsinVizag,followedbyinteractionwithcrossfunc-tionalteams(application,consumable,sales,service)overdinner.

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VOLUME 49 • Summer Edition, 2016

PerkinElmer (India) Pvt. Ltd.G-Corp Tech Park, 8th Floor, Near Hypercity Mall, Ghodbunder Road, Kasarvadavali, Thane (West) 400 615, Maharashtra, India.Tel: +91-22-3326 1700, Fax: +91-22-3326 1790, Email: [email protected] CIN No.: U74999MH2004PTC145744www.perkinelmer.com

India offices address

Head Office (Thane) PerkinElmer (India) Pvt. Ltd.G-Corp Tech Park, 8th Floor, Near Hypercity Mall, Ghodbunder Road, Kasarvadavali, Thane (West), Maharashtra 400 615 IndiaTel: +91-22-33261700

HyderabadPerkinElmer (India) Pvt. Ltd. Level 6, Building #9, RahejaMindspace, IT Park, Hi-Tech City, Madhapur, Hyderabad, Andhra Pradesh 500 081, India Tel: +91-40-39820700, +91-40-39820720

Delhi PerkinElmer (India) Pvt. Ltd.414-415-416, DLF Tower, Shivaji Marg (Moti Nagar), New Delhi 110 015, India Tel: +91-11-45006600 / +91-11-45548620, +91-11-45548622

Chennai PerkinElmer (India) Pvt. Ltd.PerkinElmer India Pvt. Ltd.Block No. 701, 7th Floor, TICEL Bio ParkPhase II, No. 5, CSIR RoadTaramani, Chennai – 600 113Tel: +91-44-66778900 / 66886370

KolkataPerkinElmer (India) Pvt. Ltd.Marlin Links, 4th Floor, 166B, S. P. Mukherjee Road, Kolkata, West Bengal 700 026, India Tel: +91-33-24631517 / 18, +91-33-24631519

Baroda PerkinElmer (India) Pvt. Ltd.903-905 Siddharth Complex, R.C. Dutt Road, Alkapuri Baroda, Gujarat 390 007, India Tel: +91-265-6643930, +91-265-6643931

MohaliPerkinElmer (India) Pvt. Ltd.Quark Media Building, A-45, Industrial Area, Phase VIII B, Mohali 160 059, Punjab, IndiaTel: +91-0172-3011936 / 37/38/39

Bengaluru PerkinElmer (India) Pvt. Ltd.No. 33, ‘SwayamPrabhe’, North Park Road, Kumara Park East, Bengaluru, Karnataka 560 001, IndiaTel: +91-80-41738989 / 41738974 +91-80-40953072

PunePerkinElmer (India) Pvt. Ltd.47/48 Patil Arcade, Opp. Sharda Center Next to Persistent Systems, Pune, Maharashtra 411 004, IndiaTel: +91-20-25437727 / 65231041, +91-20-25437727

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