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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Chemisches und Veterinruntersuchungsamt (CVUA)
Freiburg
Determination of Chloroparaffins
in Foodstuffs by GC-MS/MS
Biljana Trajkovska, Karin Kypke,
Alexander Kotz, Rainer Malisch,
Ralf Lippold
Food Testing and Agriculture Solutions
Webinar
23 October 2012
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Chemisches und Veterinruntersuchungsamt (CVUA)
Freiburg
Determination of Chloroparaffins
in Foodstuffs by GC-MS/MS
Biljana Trajkovska, Karin Kypke,
Alexander Kotz, Rainer Malisch,
Ralf Lippold
Food Testing and Agriculture Solutions
Webinar
23 October 2012
-
State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Content
Chloroparaffins:
1. Applications, regulations, levels in the food chain
2. Analytical methods for food and human milk
Extraction and clean up
GC-MS/MS
3. Results for CPs in samples of this study
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Chlorinated Paraffins (CPs) (polychlorinated n-alkanes, PCAs)
general formula CnH2n+2-zClz
chain length and the number and position of the chlorines can vary
complex mixtures: > 10.000 compounds
chlorine content of the commercially available mixtures varies between 30 70 %
CPs are divided according their carbon chain length into
short chain CPs (SCCP; C10 C13)
medium chain CPs (MCCP; C14 C17)
long chain CPs (LCCP; > C17)
Molecular Structure
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Applications of Chlorinated Paraffins (CPs)
metal industry (lubricant, cutting oil)
flame retardants in rubber, in paints, for coatings, sealants
textile industry as flame retardants, for repelling water and as anti-fouling agent
leather industry for fat liquoring
plasticiser in PVC, especially MCCP (alternative to phthalates)
Use
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
SCCP
classified as persistent
high potential for bioaccumulation
classified as toxic to aquatic organisms
carcinogenic to rats and mice
Toxicology
categorized by IARC in group 2 B
as possible carcinogenic to humans
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Directive 2002/45/EC
SCCP were banned for certain applications
- in metal and leather industry
EU Regulations
Production, the marketing and the use of SCCP is prohibited,
whether on their own, in preparations or as constituents of articles
COMMISSION REGULATION (EU) No 519/2012
and Annex I of the Regulation (EC) No 850/2004
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Stockholm Convention on Persistent Organic Pollutants (POPs)
Adopted and signed at Diplomatic Conference in Stockholm, May 2001;
Convention entered into force on 17 May 2004;
Aim:
Protection of human health and the environment
Reduction or elimination of releases of certain POPs
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Stockholm Convention on Persistent Organic Pollutants (POPs)
Comprises: Pesticides, industrial chemicals, by-products
Initial 12 POPs
New POPs (number: 10)
Candidate POPs (number: 5;
among them: Short-Chained Chlorinated Paraffins)
http://chm.pops.int
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Parties to Stockholm Convention
October 2012: 178 Parties (with152 Signatories)
http://chm.pops.int
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
CP levels in fish from Germany and Switzerland
Reth (2006): Total CP concentrations
in various fish species (muscle
tissue) captured in Germany and
Switzerland. Determination by
HRGC-EI-MS/MS:
Range 0.5 27 % lipid
Range 10 250 ng CP/g ww
Range 500 8000 ng CP/g lw
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
CP levels in human milk from Germany
Reth M, Kypke K, Schchtele J and Oehme M, Organohalogen Compounds (2005) 67:1671-1673
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
CP levels
in human milk from UK
Gareth OT, Farrar D, Braekevelt E, Stern G,
Kalantzi OI, Martin FL, Jones KC in
Environment International 32 (2006) 34 40
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Content
Chloroparaffins:
1. Applications, regulations, levels in the food chain
2. Analytical methods for food and human milk
Extraction and clean up
GC-MS/MS
3. Results for CPs in samples of this study
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Literature
35 references found with
chlorinated paraffins in titles of presentations given at the
annual dioxin conferences
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Literature
35 references found with
chlorinated paraffins in titles of presentations given at the
annual dioxin conferences
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Michael Oehme and his former workgroup at University of Basel (Switzerland):
Reth M. and Oehme M. Limitations of low resolution mass spectrometry in the electron capture negative ionization mode for the analysis of short and medium chain chlorinated paraffins Anal. Bioanal. Chem. 2004, 378, 1741-1747
Reth M., Zencak Z. and Oehme M. First study of congener group patterns and concentrations of short- and medium-chain chlorinated paraffins in fish from the North and Baltic Sea Chemosphere 2005, 58, 847-854
Z. Zencak, M. Reth and M. Oehme Determination of Total Polychlorinated n-Alkane Concentration in Biota by Electron Ionization-MS/MS Anal. Chem. 2004 76, 1957-1962
Z. Zencak, A. Borgen, M. Reth and M. Oehme Evaluation of four Mass Spectrometric Methods for the Analysis of Polychlorinated n-Alkanes J. Chromatogr. A 2005, 1067, 295-301
Scientific basis for development of analytical procedure
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Extraction and clean up:
1. fat extraction
different procedures depending on matrix and fat content
2. removal of fat
column chromatography with silica gel impregnated with sulphuric acid
3. clean up adsorption chromatography on Florisil
4. Determination by GC/MS
Analytical procedure
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Internal standards:
1.[13C10]-trans-Chlordane
2. -Hexachlorocyclo-hexane
Analytical procedure
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
samples with a high fat content for example: bacon, kidney fat
2 5 g sample
A Fat Extraction
melted fat
heated in a microwave oven
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
raw milk / human milk
50 g milk
fat extraction with n-hexane /
dichloromethane 1+1 (v+v)
solvent is removed by using a turbo vap 500
centrifuged at 4C (3000 rpm, 10 min)
homogenize the cream with
water free sodium sulphate
A Fat Extraction
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
meat / cheese / eggs
A Fat Extraction
10 g sample
lipid is extracted with n-hexane /
dichloromethane (1:1)
solvent is removed by using a Turbo Vap 500
homogenize with water free
sodium sulphate
mixture is packed into
a glass column
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
B Removal of Fat by Oxidation
glas wool
silica gel/
sulfuric acid (44 %)
Na2SO4
Na2SO4
conditioning: n-hexane / dichloromethane (1:1)
elution: n-hexane / dichloromethane (1:1)
evaporation with Turbo Vap
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
plant oil
glass wool
silica gel/
sulfuric acid (44 %)
Na2SO4
Clogging of column can be caused by compounds difficult to oxidize (e.g. waxes)
B Removal of Fat by Oxidation
conditioning: n-hexane / dichloromethane (1:1)
elution: n-hexane / dichloromethane (1:1)
evaporation with Turbo Vap
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
plant oil
glass wool
silica gel/
sulfuric acid (44 %)
Na2SO4
silica gel/
sodium hydroxide
B Removal of Fat by Oxidation
conditioning: n-hexane / dichloromethane (1:1)
elution: n-hexane / dichloromethane (1:1)
evaporation with Turbo Vap
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
C Florisil column
conditioning:
n-hexane
pre-wash:
n-hexane
dichloromethane
elution:
dichloromethane
evaporate with turbo vap
dissolve residue in
cyclohexane
glass wool
florisil
deactiviated with
1.5 % water
Na2SO4
Na2SO4
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Figure 1: mix standard solution
mix standard solution with
PCB, DDT, nonachlor
(c = 0.4 ng /l)
after clean up on Florisil
Figure 2: mix standard solution, after clean up on Florisil
C Florisil column
Separation of organochloro pesticides and PCBs from chlorinated paraffins
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Content
Chloroparaffins:
1. Applications, regulations, levels in the food chain
2. Analytical methods for food and human milk
Extraction and clean up
GC-MS/MS
3. Results for CPs in samples of this study
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
GC/low resolution EI-MS:
strong fragmentation of CPs under EI conditions (resulting mass spectra without
compound-specific information, e.g. chain length, number of chlorine atoms).
Fragments present in all CPs are below m/z 110.
Thus increased risk of interferences, high background from remaining sample.
GC-NICI-MS: (with CH4/CH2Cl2)
Advantage: nearly exclusive formation of [M+Cl]- and suppression of formation
of other fragment ions; enhances selectivity and sensitivity; allows reliable
quantification independent from degree of chlorination
Disadvantage: not suitable for routine analysis - cleaning of instrument
necessary after 48 hours
GC/HRMS
Advantage: avoids interferences from other contaminants
Disadvantage: HRMS expensive and not available in many laboratories
Options for determination of CP with GC-MS (1)
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
GC-MS/MS (EI mode)
GC-ECNI-MS
Options for determination of CP with GC-MS (2)
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Analysis of CP
CPs are complex technical mixtures with thousands of isomers
Chromatograms with broad humps instead of single peaks
Determination of all homologue groups very time-consuming
Quantification of CP extremely difficult
response factor depends on the chlorine content
Analysis of CP
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
GC-MS/MS (EI mode)
GC-ECNI-MS
Options for determination of CP with GC-MS (2)
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Determination of total concentration with GC-MS/MS (EI-mode)
EI Scan; SCCP 55.5 % Cl
m/z 110
EI Scan; MCCP 42 % Cl
m/z 110
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Determination of total concentration with GC-MS/MS (EI-mode)
Analyte Precursor Ion
(m/z)
Product Ion
(m/z)
Collision Energy
(V)
CPs 91 [C7H7]+ 53 [C4H5]
+ -16
CPs 102 [C5H7Cl]+ 65 [C5H5]
+ -10
CPs 102 [C5H7Cl]+ 67 [C5H7]
+ -18
[13C10]-trans-
Chlordane 383 [M-Cl]+ 276 [M-4Cl]+ -20
-Hexachlorocyclo-hexane
181 [M-3Cl]+ 145 [M-4Cl]+ -15
-Hexachlorocyclo-hexane
181 [M-3Cl]+ 109 [M-5Cl]+ -31
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Parameters of GC-EI-MS/MS
instrument: Agilent Technologies 7000 GC/MS Triple Quad,
7693 Autosampler, 7890A GC System
column: HP-5MS
fused silica capillary column (15 m length x 0.25 mm i.d.),
coated with 0.25 m of 5%-phenyl-methylpolysiloxane
injector temperature: 280 C
injection: splitless
injection volume: 2.5 l
transferline: 280 C
ion source temperature: 200 C
electron energy: 70 eV
carriergas: helium, constant flow of 2 ml/ min
temperature programme: 1 min isothermal at 100 C, increased at 50 C/ min to 300 C,
isothermal for 5 min
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Chromatograms of SCCP and MCCP
MCCP 57 % Cl; 102 -> 67
MCCP 57 % Cl; 102 -> 65
MCCP 57 % Cl; 91 -> 53
SCCP 55.5 % Cl; 102 -> 67
SCCP 55.5 % Cl; 102 -> 65
SCCP 55.5 % Cl; 91 -> 53
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
MCCP 57 % Cl; TIC SCCP 55.5 % Cl; TIC
SCCP 55.5 % Cl + MCCP 57 % Cl; TIC
Chromatograms of SCCP and MCCP
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
GC-EI-MS/MS
SCCP 55.5 % [102 -> 67]
SCCP 55.5 % [102 -> 65]
SCCP 55.5 % [91 -> 53]
low LODs resp. LOQs for all three transitions
Relevant range: for analysis of CPs in food between 0.5 20 ng/ l
GC-MS/MS is suitable for the
determination of CP in food
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
GC-MS/MS (EI-mode):
Allows determination of total CP concentration
Advantage
low variation of response factor (according to Zencak, quantification does
not depend on chain length and degree of chlorination.)
fast determination of total concentrations of SCCP and MCCP (possible
further characterization by ECNI-LRMS)
Disadvantage:
strong fragmentation of CPs under EI conditions gives mass spectra without
compound-specific information (e.g. chain length, number of chlorine
atoms): fragments present in all CP are below m/z 110 (thus increased risk
of interferences, high background from remaining sample)
Separate quantification of SCCP and MCCP not possible
GC-MS/MS (EI-mode)
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
GC-MS/MS (EI mode)
GC-ECNI-MS
Options for determination of CP with GC-MS (2)
published by Reth (2006)
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Chemisches und Veterinruntersuchungsamt Freiburg
Advantage
no strong fragmentation of CPs under ECNI conditions
leads to formation of [M-Cl]- as major fragment
allows the evaluation of all congener and homologue groups of SCCP and MCCP
allows a differentation between SCCP and MCCP
Determination of CPs using GC-ECNI-MS
Disadvantage
GC-ECNI-MS does not detect lower chlorinated CPs
high number of runs per sample is necessary
the quantification depends on the degree of chlorination of the used standard
GC-ECNI-MS is time consuming
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Comparability of CP levels in fish determined by ECNI-
MS and EI-MS/MS
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Comparability of CP levels in fish determined by ECNI-
MS and EI-MS/MS
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Comparability of CP levels in fish determined by ECNI-
MS and EI-MS/MS
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Method Blanks
possible sources causing contamination in laboratory:
glassware CP bind to active surface
technical equipment (in contact with samples or extracts)
chemicals
air (air condition)
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Method Blanks
measures to reduce the risk of contamination during clean up
Soaking of glassware in detergent solution
Heating of glassware up to 450 C for 2 hours
Covering of glassware in alumina foil for storage and during analysis
Rinsing of glassware with solvent immediately before use
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Method Blanks
blank values shall be below 0.1 ng/ l (corresponding to 5 ng/g lipid with use of the
established method)
Measures to reduce the risk of contamination during clean up
no plastic materials
teflon cleaned with solvent for use
heating of chemicals at 600 C overnight
use only of high purity solvents
extraction of glass wool with solvent
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Validation of the Matrix Raw Milk
Level 1
[2 ng/g]
Recovery
[%] Level 2
[10 ng/g]
Recovery
[%]
Sample 1 1.82 91 9.50 95
Sample 2 1.66 83 10.0 100
Sample 3 1.46 73 9.30 93
Sample 4 2.42 121 9.74 97
Sample 5 2.06 103 11.7 117
number of samples 5 5
mean [ng/ l] 1.88 94 10.1 101
standard deviation [ng/ l] 0.19 0.49
rel. standard deviation [%] 20 10
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
xblind = 0.12 ng/ l
sblind = 0.05 ng/ l
LOD = 0.26 ng/ l
LOQ = 0.60 ng/ l
LOD = xblind + 3 * sblind
LOQ = xblind + 10 * sblind
Calculation of LOD and LOQ depending on blank value:
Collection of results of individual blank values over a period of 3 month
Calculation of mean and standard deviation from these collected data
Validation of the Matrix Raw Milk
LOD = 0.5 ng/ g milk
LOQ = 1.2 ng/ g milk
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Content
Chloroparaffins:
1. Applications, regulations, levels in the food chain
2. Analytical methods for food and human milk
Extraction and clean up
GC-MS/MS
3. Results for CPs in samples of this study
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Samples
mirco1 / pixelio.de
Peter Hebgen / pixelio.de Matthias Koranzki / pixelio.de
Samples analysed:
10 samples of raw milk
10 samples of cheese
25 samples of human milk
4 samples of wild boar
6 samples of meat
6 samples of plant oil
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Raw Milk
pooled samples of
severals farms CP
[ng / g fat]
CP [ng / g wet weight]
raw milk 1 Tour I < LOD < LOD
raw milk 2 Tour 13 < LOD < LOD
raw milk 3 Tour 7 < LOD < LOD
raw milk 4 Tour 6 < LOD < LOD
raw milk 5 Tour 8 < LOD < LOD
raw milk 6 Tour 1 < LOD < LOD
raw milk 7 Tour 12 < LOD < LOD
raw milk 8 Tour Ellrich < LOD < LOD
raw milk 9 Tour Frankenhardt < LOD < LOD
raw milk 10 Tour Eckartshausen < LOQ [26] < LOQ [1.0]
Chloroparaffins LOD: 13 ng/ g fat LOQ: 30 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Raw Milk
SCCP 55.5 % chlorine content MCCP 57 % chlorine content
raw milk sample 10
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Cheese
lipid
content
[%]
CP [ng / g fat]
CP [ng / g wet
weight]
country of
origin
animal
1 Brie 24,1 41 5.0 The Netherland organic goat
2 Feta cheese 24,4 122 24 Greece organic sheep and
goat
3 Feta cheese 26,2 94 19 Germany organic sheep
4 Feta cheese 28,4 38 7.5 Germany organic sheep
5 Cheese 26,5 < LOQ [18] < LOQ [3.6] France conventional cow
6 Mozzarella 21,0 55 11 Italy conventional buffalo
7 Cheese 32,0 < LOQ [28] < LOQ [5.5] Italy organic sheep
8 Feta cheese 22,7 47 9.3 Greece organic sheep
9 Goat cheese 27,1 42 8.4 Germany organic goat
10 Goat cheese 27,8 < LOQ [18] < LOQ[3.6] Germany organic goat
Chloroparaffins LOD: 13 ng/ g fat LOQ: 30 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Cheese
lipid
content
[%]
CP [ng / g fat]
CP [ng / g wet
weight]
country of
origin
animal
1 Brie 24,1 41 5.0 The Netherland organic goat
2 Feta cheese 24,4 122 24 Greece organic sheep and
goat
3 Feta cheese 26,2 94 19 Germany organic sheep
4 Feta cheese 28,4 38 7.5 Germany organic sheep
5 Cheese 26,5 < LOQ [18] < LOQ [3.6] France conventional cow
6 Mozzarella 21,0 55 11 Italy conventional buffalo
7 Cheese 32,0 < LOQ [28] < LOQ [5.5] Italy organic sheep
8 Feta cheese 22,7 47 9.3 Greece organic sheep
9 Goat cheese 27,1 42 8.4 Germany organic goat
10 Goat cheese 27,8 < LOQ [18] < LOQ[3.6] Germany organic goat
Chloroparaffins LOD: 13 ng/ g fat LOQ: 30 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Cheese
SCCP 55.5 % chlorine content MCCP 57 % chlorine content
Feta cheese, greece
122 ng/ g CP
Feta cheese, germany
94 ng/ g CP
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human milk is particulary well suited for biomonitoring of POPs
easy way to get high fat content
Study was organised by WHO and UNEP with CVUA Freiburg as
Reference Laboratory.
The study is performed as contribution to the Stockholm Convention.
The aim is to get comparable data for the background concentration of
POPs and for evaluation of time trends.
Each country participating in the study sent one representative sample
prepared by pooling (mixing) of at least 50 individual human milk
samples.
Human Milk
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
23 500 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
Asia
Europe Pacific Island
Conc. [ng/ g fat]
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
Asia
Europe Pacific Island
3026 ng/ g fat 8492 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
Conc. [ng/ g fat]
-
State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Human Milk
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Wild Boar
Sample
age
[month]
CP
[ng/ g fat]
HCB
[ng/ g
fat]
alpha-HCH
[ng/ g fat]
beta-HCH
[ng/ g fat]
lindane [ng/
g fat]
1 wild boar, fat 12 < LOQ [18,1] 951 < LOD < LOD < LOD
2 wild boar, fat 12 < LOQ [17,3] 8.4 2.9 23.0 < LOD
3 wild boar, fat - < LOQ [29,8] 14.2 78.1 54.1 < LOD
4 wild boar, fat 12 < LOQ [26,2] 12.9 12.4 5.9 < LOD
maximum amount by law - 200 200 100 20
Chloroparaffins
LOD: 13 ng/ g fat
LOQ: 30 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Meat
CP [ng/ g fat] country of origin
1 chicken < LOQ [26] Germany
2 turkey < LOD Germany
3 goose 34 Germany
4 beef < LOQ [33] Germany
5 beef 60 Germany
6 beef < LOQ [28] Germany
Chloroparaffins
LOD: 13 ng/ g fat
LOQ: 30 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Meat
SCCP 55.5 % chlorine content MCCP 57 % chlorine content
beef
60 ng/ g fat CP
goose
34 ng/ g fat CP
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Olive Oil
CP [ng/ g fat]
1 olive oil < LOD
2 olive oil 75
3 olive oil < LOQ [20]
4 olive oil 98
5 olive oil 38
6 olive oil 37
LOD: 13 ng/ g fat
LOQ: 30 ng/ g fat
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Outlook
Actual activity:
Determination of CPs with GC-ECNI-MS as second type of
detection
for comparison of results of both ionization
techniques (confirmation)
for determination of CP patterns
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State Institute for Chemical and Veterinary Analysis of Food
Freiburg (Germany)
Final
Thank you for your attention
Patricia Fischer,
Sebastian Schelb,
Katrin Thoma,
Nadine Singler