decontamination of cosmetic products and raw materials by...

198

FABAD J. Pharm. Sci., 31, 198-209, 2006

RESEARCH ARTICLE

Decontamination of Cosmetic Products and Raw Materials by Gamma IrradiationSummary

Decontamination of Cosmetic Products andRaw Materials by Gamma Irradiation

In this study, we aimed to use gamma irradiation for decontamination of cosmetic products in order to achieve the acceptable microbiological limits. Cosmetic products and raw materials were irradiated (5-7.5-10 kGy) and physicochemical, microbiological and biological properties of these samples were evaluated in normal and stress storage conditions. It was found that the physicochemical properties of samples tested were changed after irradiation. No change was observed in skin irritation properties of all samples tested. Decontamination dose for all samples, excluding starch, was found to be about 5 kGy or below. Key Words: Decontamination by gamma radiation, cosmetic products, cosmetic raw materials.Received : 03.03.2008Revised : 27.03.2008Accepted : 29.05.2008

* Hacettepe University, Faculty of Pharmacy, Department of Radiopharmacy, 06100, Ankara,Turkey. ** Hacettepe University, Faculty of Pharmacy, Department of Pharmaceutical Microbiology, 06100, Ankara, Turkey.*** Hacettepe University, Faculty of Medicine, Department of Dermatology, 06100, Ankara, Turkey.**** Hacettepe University, Faculty of Engineering, Department of Physics Engineering, 06532, Ankara, Turkey.° Corresponding author e-mail : [email protected]

INTRODUCTION

Gamma irradiation has an increasingly important

role in the manufacture of cosmetic products [1]. The

use of gamma rays is an alternative method for ster-

ilization/decontamination of products and raw ma-

terials [2]. However, one of the major problems of

irradiation is the occurrence of new radicals during

the process [3]. Irradiation is never a substitute for

poor compliance to Good Manufacturing Practice

(GMP) guidelines. In fact, it should be a part of GMP

[4]. The gamma radiation process cannot make some-

thing radioactive or leave any residual radioactivity.

Microorganisms are killed either as a result of the

destruction in a vital molecule or by chemical reaction

of compounds resulting from radiation. The most

widely used application of gamma radiation process-

ing is in the control of microbial contamination levels

[1].

Topically applied preparations must not contain mi-

crobials exceeding the permissible limits. This is

199

achieved through the decontamination and steriliza-

tion process [5]. In many cases, the offending organ-

isms in a cosmetic product are Escherichia coli (E.

coli) or Pseudomonas aeruginosa (P. aeruginosa).

Both are especially susceptible to radiation energy at

very low doses, which often means that the radiation

effect on the product is negligible [6]. Cosmetic prod-

ucts may be contaminated during manufacturing by

microorganisms existing in the environment or in the

raw materials. Raw materials, especially water, found

in most of the cosmetic preparations form an appro-

priate media for microbial growth. There is no certain

radiation dose level in pharmacopoeia and guidelines

for decontaminating cosmetic preparations and cos-

metic raw materials. However, acceptable microbio-

logical limits are recommended in guidelines for a

variety of cosmetic preparations. These limits are

between 102 and 103. Generally, the gamma radiation

dose preferred to achieve these levels ranges between

5 and 15 kGy. 60Co source, which is commonly used

for gamma irradiation, can be used for cosmetic raw

materials and finished products. Aiming at the reduc-

tion in microbiological content, the method does not

leave any residues that may be harmful to the em-

ployees or consumers. Gamma radiation can penetrate

the packaging materials and sealed packages contain-

ing the finished products, thus destroying the existing

microorganisms. Decontamination by gamma radia-

tion is gaining increasing attention in cosmetic pro-

duction.

MATERIALS and METHODS

Materials used in the experiments are coded in Table

1. A, B, and C were kindly provided from Colgate-

Palmolive, D from Canan Kozmetik, E, F, G, H, I, J,

K, L from Eczac›bafl›-Beiersdorf, M from Evyap, N,

O, P from Eczac›bafl›-Avon, R from Johnson & Johnson,

S, V, Y from Merck, T from Roquette Freres, and U

from Çapamarka.

Statistics

Physicochemical test results are given as the mean of

6 experiments; whereas, n = 3 was applied for biolog-

ical and microbiological tests. Kruskal-Wallis and

non-parametric Mann-Whitney U tests were used as

the significance tests and SPSS computer software

program was employed for analyses.

Irradiation Process

Irradiation was performed at room temperature using

a 60Co Gamma Cell 220 available at the Turkish Atomic

Energy Agency (TAEK) at a dose rate of 2.84 kGy h-

1. All samples in glass vials were irradiated at doses

of 5, 7.5, 10 kGy. Bioburden and irritation tests were

carried out for sample K.

Unirradiated samples were used as controls to detect

physicochemical, biological and microbiological

changes resulting from the action of ionizing radiation

on the cosmetic products and raw materials investi-

gated. Experiments performed on cosmetic samples

are summarized in Table 2.

Physicochemical Properties

All tests were performed on unirradiated samples

and samples irradiated at doses of 5, 7.5 and 10 kGy

(Table 2). Results were analyzed statistically.

Table 1. Codes of materials used

Cosmetic Cosmetic Cosmetic Raw

Code Product Code Product Code Materials

A Baby powder J Concealer S Talc

B Solid soap K Mascara T Wheat starch

C Solid soap L Eye pencil U Corn starch

D Liquid soap M Solid soap V Bentonite

E Baby powder N Redness Y Gelatin

F Lush on O Lip pencil

G Compact powder P Foundation

H Foundation R Baby powder

I Eye shadow

Table 2. Tests performed on cosmetic samples under normal conditions

COSMETIC PRODUCTS

Physicochemical Tests

Biological Test

- Irritation test

Microbiological Tests

- Bioburden

- Determination of decontamination dose

Solid and liquid soaps

- Organoleptic properties

- pH

- Viscosity

- Foam height

Other preparations


- Particle size

COSMETIC RAW MATERIALS


Biological Test

- Irritation test

Microbiological Tests

- Bioburden

- Determination of

decontamination dose


- Particle size

- ESR behavior

200

FABAD J. Pharm. Sci., 31, 198-209, 2006

-Organoleptic Properties: Solid and liquid soaps were

evaluated by their color, odor and general appearance.

-pH: [5% (w/v)] solutions of unirradiated and irradi-

ated soaps were prepared and pH of these solutions

were measured at room temperature (25°C) and at

40°C (Sesa Model 1400).

- Viscosity: Viscosities of unirradiated and irradiated

1% (w/v) soap solutions were measured by Brookfield

rheometer (DV-II model) at two different temperatures

of 25°C and 40°C.

-Foam Height: To determine the foam height, 5 ml of

unirradiated and irradiated 1% (w/v) soap solutions

were placed in tubes and vigorously shaken for 10

min at 280 rpm.min-1. Foam height was calculated as

the ratio of foam height to total height. The same

procedure was repeated at 25°C and 40°C.

-Mean Particle Size and Distribution: Unirradiated

samples and samples irradiated at doses of 5, 7.5 and

10 kGy were investigated. Mean particle sizes and

size distributions of cosmetic samples except soaps,

i.e. foundations, concealer, mascara, eye pencil and

lip pencil, were measured by laser diffraction method

(Sympatec Helos (H 0728) Particle Size Analyzer).

-ESR Behavior: Electron spin resonance (ESR) studies

were done on cosmetic raw materials before and

immediately after irradiation. These studies were

carried out using a Varian 9”E-LX Band ESR Spec-

trometer. Each spectrum was corrected for variation

using the amount of material in the ESR tube.

Microbiological Properties

The neutralization process of antimicrobial property

was not validated because the aim of this research

was to determine the bioburden of cosmetic raw

materials and products and to compare these findings

with the limits permitted legally. The purpose was to

find the reliability of cosmetic products and raw

materials available on the Turkish market and in

accordance with the guidelines.

In order to obtain these results, 1 g of cosmetic product

or raw material was used in the experimental part

and all samples were contaminated with Bacillus

pumilus spores (106 cfu.mL-1) at the beginning of the

study.

-Bioburden: In order to determine the microbial load

(bioburden) of samples, 1 g of each sample was

weighed in sterile vials and 1 ml of sterile distilled

water was then added. Each mixture was mixed for

1 min; 0.1 ml of samples were withdrawn from vials

and inoculated on plates with tryptic soy agar. All

plates were incubated for 24-48 h at 37°C followed

by counting the number of colonies with naked eye.

-Determination of Decontamination Dose Level:

Samples were contaminated by the most radiation-

resistant microorganism, Bacillus pumilus spores (106

cfu.mL-1), in order to determine the decontamination

dose level. The samples were then irradiated at dif-

ferent dose levels of 2, 5, 7.5 and 10 kGy. Each sample

was mixed for 1 min; 0.1 ml of samples were with-

drawn from vials and inoculated on plate with tryptic

soy agar. All plates were incubated for 24-48 h at 37°C,

followed by counting the number of colonies with

naked eye.

Biological Properties

-Irritation Test: Possible irritation effects of unirradi-

ated and irradiated samples were evaluated using

occlusive patch test. Patches were applied to the

forearms of healthy volunteers. Patches were removed

24 h later, and forearms were washed with tap water.

Irritation was evaluated by a dermatologist using the

scores given in Table 3. The test was repeated 3 times

Table 3. Scoring of irritation

Erythema0 No evidence of erythema0.5 Minimal or doubtful erythema1 Slight, spotty and diffuse redness2 Moderate, uniform redness3 Strong uniform redness4 Hot rednessDryness0 No evidence of scaling0.5 Dry without scaling; appears smooth and tight1 Fine/mild scaling2 Moderate scaling3 Severe scaling with large flakesEdema- Absence of edema+ Presence of edema

201

per sample. In total, 18 healthy volunteers were used

for 22 samples.

5% (w/v) soap solutions were used for this test. 15

mg of samples A, E, F, G, H, I, N and R were weighed

and placed in the Finn chambers. One drop of samples

H and P were absorbed on special filter papers, and

then placed in the chamber. For sample K, 2 ml of

distilled water was added to the original package

and mixed for 2 min; then, one drop of mixture was

put on special filter paper and then placed in the

chamber. A certain amount of samples J, L and O

were placed in chambers. At the end of the test, the

score table (Table 3) [7] was used for evaluating the

results.

Stability Studies

In this part of the study, tests performed for samples

under normal environmental conditions were repeated

with samples stored in unsealed glass tubes for cos-

metic raw materials and in sealed glass tubes for

cosmetic products, at high temperature (40±2)ºC and

high relative humidity (75±5)% conditions over a

period of 3 months. Possible changes wer e investigat-

ed at accelerated conditions after irradiation. Exper-

imental studies carried out for this purpose are sum-

marized in Table 4.

- ESR Behavior: Peaks obtained in the ESR studies in

normal environmental conditions were also evaluated

in the samples at the end of the stability studies to

determine any radical formation.

RESULTS and DISCUSSION

Studies Carried Out Under Normal Conditions

Physicochemical Properties

Physicochemical properties of soaps treated with

gamma radiation are widely described, but not for

other cosmetics. Therefore, physicochemical tests

were applied to cosmetic products considering the

existing guidelines or other official sources. For those

properties not officially mentioned, particle size mea-

surements, organoleptic properties and ESR studies

were considered as sufficient.

- Organoleptic Properties: Organoleptic properties

of unirradiated and irradiated soaps are summarized

in Table 5. It was determined that there was no change

in the organoleptic properties of soap samples irradi-

ated at the 3 different doses.

- pH: pH values of soaps were found to change after

irradiation at all 3 doses. Changes in pH values of all

soaps seem to be independent from irradiation dose

levels (p>0.05). Results are given in Table 6.

Table 4. Physicochemical tests performed on cosmetic products and raw materials during the stability studies

COSMETIC PREPARATIONS


Solid and liquid soaps

-Organoleptic properties

-Viscosity

-pH

-Foam height

Other preparations


-Particle size

COSMETIC RAW MATERIALS



-Particle size

Table 5. Organoleptic properties of liquid and solid soaps before and after irradiation

Code

BCDM

Unirradiated

Blue/light blue barOrange, transparent bar

White, opaque liquidYellow/light yellow bar

Dose (kGy)

5++++

7.5++++

10++++

Organoleptic Properties

(+ : no change; - : change)

Table 6. pH values of unirradiated and irradiated soaps at two different temperatures

Code

B

C

D

M

* value represents mean ± standard deviation, n=6.

Temperature

(°C)

25

Unirradiated

9.31±0.01

9.15±0.02

6.11±0.04

9.39±0.02

5

9.45±0.04

9.29±0.02

6.05±0.08

9.45±0.02

7.5

9.64±0.03

9.48±0.04

5.87±0.04

9.71±0.03

10

9.69±0.03

9.54±0.04

5.95±0.04

9.65±0.02

Statistical

Evaluation

p<0.05

p<0.05

p<0.05

p<0.05

Dose (kGy)

pH

40

Unirradiated

9.25±0.09

9.18±0.05

6.04±0.07

9.20±0.04

5

9.41±0.03

9.23±0.02

5.88±0.05

9.42±0.02

7.5

9.48±0.05

9.42±0.02

5.85±0.05

9.61±0.04

10

9.30±0.03

9.13±0.02

5.78±0.04

9.29±0.04

Statistical

Evaluation

p<0.05

p<0.05

p<0.05

p<0.05

Dose (kGy)

pHCode

B

C

D

M

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FABAD J. Pharm. Sci., 31, 198-209, 2006

pH values of solid soaps B, C and M increased with

the increase in radiation dose levels. However, pH

value of liquid soap D decreased with the increase in

irradiation dose. These differences in pH values may

be attributed to the trace amount of radicals formed

by irradiation. Results obtained in this study are in

agreement with the literature, since it was reported

that decrease in the pH value of an antibacterial agent

after irradiation was found to be independent of the

irradiation dose levels [8,9].

- Viscosity: Inconsistent results were obtained from

viscosity measurements of solid soaps at 25°C due to

the gel formation at room temperature (data not

presented). Therefore, viscosity measurements of solid

soaps were performed only at 40°C while viscosities

of liquid soaps were measured at 25°C and 40°C.

Viscosities of unirradiated solid soaps (B, C, M) and

those irradiated at the 3 different doses did not change

significantly at 40°C (p<0.05). There were significant

(p<0.05) differences in viscosities of unirradiated

liquid soaps compared with samples irradiated at the

3 different doses at both temperatures. According to

these results, it can be concluded that solid soaps are

more stable against irradiation than liquid soaps.

Results are given in Figure 1 a-d. Jacobs et al. [10]

reported changes in viscosities of some materials after

irradiation. For example, viscosity of tragacanth gum

was decreased with increasing radiation dose [10]. In

another study, application of radiation dose between

5 and 15 kGy on HPMC (hydroxypropyl methylcel-

lulose) powder solution displayed pseudo-plastic

behavior at the beginning followed by a Newtonian

flow. Viscosity of HPMC solution was decreased with

an increase in the irradiation dose (5-15 kGy) [11].

- Foam Height: Although foaming of soaps or deter-

gents is independent from their cleansing properties,

it is perceived as the sign of cleanliness due to psy-

chological factors. Foam heights of soaps were found

to change after irradiation. The results obtained

showed that the changes in foam heights of all soaps

were independent of radiation dose. Results are given

in Table 7.

- Mean Particle Size and Distribution: Mean particle

sizes of cosmetic samples irradiated at the 3 different

doses (5, 7.5, 10 kGy) were determined to change

Table 7. Foam heights of solid and liquid soaps before and after irradiation

Code

B

C

D

M

* value represents mean ± standard deviation, n=6.

Temperature

(°C)

25

Unirradiated

51.6±4.0

63.0±7.0

52.6±4.0

63.8±3.0

5

67.8±3.0

61.6±4.0

54.2±6.0

56.3±3.0

7.5

60.1±6.0

60.2±4.0

46.1±4.0

70.8±7.0

10

62.4±4.0

53.0±7.0

56.5±4.0

55.2±1.0

Statistical

Evaluation

p<0.05

p<0.05

p<0.05

p<0.05

Dose (kGy)

Foam Height (%)

40

Unirradiated

65.3±3.0

60.7±5.0

55.5±2.0

77.5±2.0

5

58.9±4.0

64.2±2.0

44.1±2.0

81.3±1.0

7.5

61.5±4.0

51.3±3.0

47.5±2.0

65.1±1.0

10

72.2±2.0

54.2±4.0

44.0±3.0

47.5±2.0

Statistical

Evaluation

p<0.05

p<0.05

p<0.05

p<0.05

Dose (kGy)

Foam Height (%)Code

B

C

D

M

Figure 1 a-d. Flow curves of solid and liquid soaps before and after irradiation at 40C (n=6).

(b)

(c)

(d)

203

when compared with the results of unirradiated

samples (p<0.05). Results of particle sizes are shown

in Figure 2 a-b.

Changes in mean particle sizes by irradiation were

observed for cosmetic products and raw materials.

Particle sizes may be different because of the changes

in forces regulating the particles in a powder [12].

However, it is not clear whether these changes are

dependent or independent of radiation since samples

did not show homogeneous particle size distribution.

- ESR Studies: ESR studies were performed only on

cosmetic raw materials. ESR spectra of unirradiated

and irradiated samples were measured under the

same conditions. No by-product peaks were detected

in unirradiated and irradiated talc and bentonite

samples. No peaks were observed for gelatin, corn

and wheat starch before irradiation. ESR spectra of

irradiated samples are given in Figures 3, 4 and 5.

Peak-to-peak intensities were determined from ESR

spectra and dose-response curves were plotted (Fig.

6 a-c). Formation of similar radicals was found on

evaluating the ESR spectra of corn and wheat starch

after irradiation. This is expected because the type

and structure of the two starches are similar.

A simulation study based on possible radical species

formation was also performed and hydroxyalkyl and

aldehydalkyl radicals were detected. These results

are in agreement with the literature since hydroxyalkyl

and aldehydalkyl radicals were determined after

irradiation of wheat, lentil and broad bean, which

contain a high amount of starch [13,14]. Suggested

radicals resulting from simulation studies are shown

in Figure 7 (for A and B) and spectroscopic parameters

are given in Table 8.

Evaluating the chemical structure of gelatin, formation

of R-CHO• (radical C) and •H (radical D) may occur

due to the degradation of CHOH by irradiation.

Simulation studies were also carried out for gelatin,

and possible radicals and their spectroscopic param-

eters are summarized in Table 9. Based on simulation

Figure 2 a-b. Mean particle size and size distribution of cosmetic products and cosmetic raw materials before and after irradiation (n=6).

(a)

(b)

Figure 3. Experimental and theoretical ESR spectra of wheat starch.

Figure 4. Experimental and theoretical ESR spectra of corn starch.

Figure 5. Experimental and theoretical ESR spectra of gelatin.

204

FABAD J. Pharm. Sci., 31, 198-209, 2006

studies, the suggested radicals are shown in Table 9

and Figure 5.

Microbiological Properties-Bioburden: Cosmetic products and ingredients may

sometimes have high bioburden. The product should

be free, as much as possible, from microbial contam-

ination, i.e. from bioburden. Generally, the lower the

bioburden, the greater is the margin of safety [15]. As

seen in Table 10, microbiological growth was observed

in samples D, F, H, J, L, N, O, P, R, S, T, U, V and Y,

while no microbial growth was observed in samples

B, C, G, I, K and M. These results may be attributed

to the general belief that solid soaps (B, C and M) are

not appropriate media for microbial growth and

production of B, C, G, I, K and M were under accept-

able GMP conditions.

- Decontamination Dose: Microbial amounts in sam-

ples after irradiation are given in Table 11. According

to the results determining the decontamination dose,

decontamination dose of all samples except corn and

wheat starches was determined to be below or around

Figure 6 a-c. Dose-response curves of a: wheat starch, b: corn starch, c: gelatin (n=6).

Table 8. ESR spectroscopic parameters resulting from simulation studies for corn and wheat starches

ParameterI

Γ(Gauss)A(Gauss) (Hβ1)A(Gauss) (OH)A(Gauss) (Hβ2)

GI

Γ(Gauss)A(Gauss) (H)

G

Corn starch92.1453.235813.3055.03685.03742.002953.9543.744035.7862.0029

Wheat starch171.0503.481213.3084.87824.86182.002992.7733.955836.8582.0028

Radicals

A

B

I: Intensity Γ : Half-width. g: Spectroscopic splitting factor. A: Hyper-fine splitting constant.

Figure 7. Suggested radicals of corn and wheat starches A: hydroxyalkyl B: aldehydalkyl.

(a)

(b)

(c)

Table 9. ESR spectroscopic parameters and radicals for gelatin

RADICALS

C

R-CHO•

D

•H

I: Intensity. Γ: Half-width. g: Spectroscopic splitting factor, A: Hyper-fine splitting constant.

PARAMETERS

I

Γ(Gauss)

A(Gauss) (proton at CHO)

A(Gauss) (proton at CH2)

A(Gauss) (proton at CH2)

g

I

Γ(Gauss)

A(Gauss)

g

GELATIN

127.660

3.6672

13.872

4.9174

4.327

2.0028

46.941

5.8685

38.840

2.0031

205

5 kGy. Decontamination dose of corn and wheat

starches was determined to be about 7 kGy. Starches

provide more appropriate conditions for microbial

growth due to their hygroscopic structure. Therefore,

decontamination dose of starches was found to be

higher than of the other samples.

Survival rates of microorganisms versus dose levels

were plotted on a logarithmic scale and the results

are given in Figure 8.

Biological Properties

- Irritation Properties: Results obtained in irritation

tests were evaluated according to Score Table (Table

3) and are given in Table 12. It was found that irritation

properties of all samples did not change after irradi-

ation (p>0.05).

Table 10.Bioburden of samples (normal microflora of cosmetic samples)

Code

A

B

C

D

E

F

G

H

I

J

K

Amount of

Microorganism (cfu.mL-1)

50

0

0

10

40

10

0

60

0

20

0

Code

L

M

N

O

P

R

S

T

U

V

Y

Amount of

Microorganism (cfu.mL-1)

50

0

120

10

50

30

>3000

1800

40

>3000

170

Table 11.Amount of microorganisms in samples before and after irradiation

Code

A

B

C

D

E

F

G

H

I

J

L

M

N

O

P

R

S

T

U

V

Y

Unirradiated

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

106

2 kGy

250

-

-

-

290

240

820

-

620

170

170

-

-

-

-

-

-

-

-

310

240

5 kGy

80

0

0

80

190

10

140

730

160

80

30

0

30

300

300

380

200

870

610

130

40

7.5 kGy

0

0

0

20

0

0

0

30

0

0

0

0

20

10

40

10

10

120

250

0

0

10 kGy

0

0

0

0

0

0

0

20

0

0

0

0

0

0

0

0

0

20

30

0

0

Microbial Amount (cfu.mL-1)

* All samples were contaminated by Bacillus pumilus spores (106 cfu/ml).

A:

D:

E:

F:

G:

206

FABAD J. Pharm. Sci., 31, 198-209, 2006

H:

I:

J:

L:

N:

O:

P:

R:

S:

T:

U:

207

Stability Studies

Organoleptic properties of samples irradiated at the

3 different doses were not changed, as with the sam-

ples stored under normal conditions. There were

differences in pH, viscosity, foam height, and mean

particle size values independent of irradiation doses

(p<0.05). This result was also the same as with the

samples stored under normal conditions.

With regard to ESR behavior, no external peaks were

detected for gelatin, corn and wheat starches on the

90th day.

CONCLUSIONS

The use of gamma radiation for decontamination is

advantageous for finished cosmetic products as well

as raw materials. Sterilization is not an obligation for

cosmetic products. However, they have to be protected

from any contamination or deterioration. This is

particularly important for the cosmetic products used

for the eyes and mouth or for babies.

Conventional cosmetic products contain carbohy-

drates, sugars, fatty acids, alcohols, starches, proteins,

amino acids, glycosides, steroids, peptides, vitamins

and some herbal ingredients in their formulations.

Figure 8. Survival-dose rates of all cosmetic samples (coded as A-Y).

V:

Y:

Table 12.Results of irritation test

Code

A

B

C

D

E

F

G

H

I

J

K

L

M

N

O

P

R

S

T

U

V

Y

EvaluationErythemaDrynessEdema

ErythemaDrynessEdema





















0 kGy0.33±0.58

0-

0.5±0.50-

1.33±0.580-

0.5±00.5±0

-00-00-00-00-00-00-00-

0.17±0.290-

0.33±0.580-00-00-00-00-00-00-00-00-00-

5 kGy0.67±1.15

0-

0.17±0.290-

0.17±0.290-00-00-00-00-00-00-00-00-

0.17±0.290-

0.33±0.580-00-00-00-00-00-00-00-00-00-

7.5 kGy00-00-

0.17±0.290-00-00-00-00-00-00-00-00-

0.17±0.290-

0.33±0.580-00-00-00-00-00-00-00-00-00-

10 kGy00-

0.17±0.290-

0.17±0.290-00-00-00-00-00-00-00-00-00-00-00-00-00-00-00-00-00-00-00-

StatisticalEvaluation

p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05p>0.05

Clinical Score

208

FABAD J. Pharm. Sci., 31, 198-209, 2006

Additionally, modern cosmetic products contain sev-

eral sensitive raw materials such as minerals, hor-

mones and enzymes. All these raw materials are

potential nutrition media for the growth of microor-

ganisms. Therefore, contamination can easily occur

as [16]:

a) Raw material contamination and b) Product con-

tamination.

For raw material contamination, ingredients within

the formulation and packaging materials are the main

contamination sources. Industrial water is a major

challenge in this sense. Starches in particular are

hygroscopic raw materials and as potential media for

the microorganisms, can easily create problems in

storage. The indications of contamination may be gas

formation and changes in color, odor, viscosity, particle

size, and pH. These organoleptic properties should

be followed although this is sometimes time-

consuming.

Product contamination is the result of production

processes originating from equipment, environment

or staff. Insufficient cleaning and disinfection of

equipment and contaminated environment or person-

nel are the factors leading to product contamination.

Gamma irradiation of raw materials decreases the

contamination risk of finished products and thus the

cost. Therefore, physicochemical properties of raw

materials are the predictions of GMP conditions of a

production process.

In this study, no significant change was determined

in organoleptic properties of raw materials S, T, U, V

and Y. Mean particle sizes of T, U and V were affected

by gamma irradiation. T and U are the starches and

due to their hygroscopic character, the particles get

agglomerated and the sizes increased. V, bentonite,

is also another hygroscopic ingredient and showed

similar behavior. Some radicals causing radiolysis

(originating from hygroscopic property) were deter-

mined by ESR studies; however, no significant changes

were found in the raw materials.

According to the physicochemical tests, no change

was observed in the organoleptic properties of soap,

make-up products, baby powders and raw materials

after irradiation. However, pH, viscosity and foam

height of soaps irradiated at the 3 different doses

were changed when compared with the unirradiated

samples. Similarly, mean particle sizes of irradiated

make-up products, baby powders and raw materials

were changed.

When the bioburden of all cosmetic raw materials

and finished products was investigated, product N

and raw materials S and V were found to have very

high microbiological loads when compared to the

official limitations (Turkish Ministry of Health Guide-

line Limitations, EC Directive-DOC XI/40517/76).

The other products and raw materials were found in

conformity with the limits.

No difference was observed between the irritation

scores produced by unirradiated and irradiated sam-

ples. Decontamination dose required to decrease the

bioburden of all samples was found to be about 5

kGy while it was around 7 kGy for the starches.

Starches provide more convenient media for microbial

growth than the other cosmetic raw materials and

products due to their hygroscopic character. Therefore,

decontamination dose for starches was found to be

higher than for the other samples. Potential for change

in the product increases with an increase in irradiation

dose. It was concluded that 5kGy was the optimal

gamma irradiation dose for decontamination purposes

for all products and raw materials, except for wheat

and maize starches.

Cosmetic products and raw materials tested in this

study, except talc and bentonite, and produced locally

or imported seem to be prepared according to the

GMP guidelines.

As a result, it can be concluded that steriliza-

tion/decontamination using gamma radiation is an

alternative method for decontamination of cosmetic

products and raw materials. Gamma radiation can

also be used much more extensively in the cosmetic

field, especially in the field of bulk raw materials.

209

Furthermore, gamma irradiation is a clean and non-

residual technology that is environmentally friendly

and safe for both employee and the community.

ACKNOWLEDGEMENTS

We wish to express our gratitude to ‹.E. Ulagay for

supplying some of the chemical materials. This study

was supported by H.U. Research Foundation (Project

No: 01.01.301.006).

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