SN/T 2106-2008 PDF English
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Determination of methylisothiazolinone and chloromethylisothiazolinone in cosmetics for import and export. Liquid chromatography
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SN/T 2106-2008: PDF in English (SNT 2106-2008) SN/T 2106-2008
SN
Industry Standard of Entry-Exit Inspection and
Quarantine of the People's Republic of China
Determination of methylisothiazolinone and
chloromethylisothiazolinone in cosmetics for
import and export - Liquid chromatography
ISSUED ON. JULY 17, 2008
IMPLEMENTED ON. FEBRUARY 1, 2009
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People’s Republic of China
Table of Contents
Foreword ... 3
1 Scope .. 4
2 Principle ... 4
3 Reagents and materials ... 4
4 Instruments ... 5
5 Determination procedure ... 5
6 Results calculation .. 6
7 Low limit of the determination .. 7
8 Recovery rate and precision ... 7
Appendix A (Informative) Liquid chromatogram of standard substance .. 8
Determination of methylisothiazolinone and
chloromethylisothiazolinone in cosmetics for
import and export - Liquid chromatography
1 Scope
This Standard specifies the liquid-chromatography determination for the
methylisothiazolinone (MIT) and chloromethylisothiazolinone (CIT) in cosmetics. This
Standard is applicable to the determination of the methylisothiazolinone and
chloromethylisothiazolinone in skin-cleaning cosmetics and skin-care cosmetics.
2 Principle
Use ultrasound to extract the methylisothiazolinone and chloromethylisothiazolinone in
cosmetics with methanol; Perform centrifugal filtration; adopt the high-performance liquid
chromatography to conduct separation and determination. Use the retention time for
qualitativeness; use the external standard method for quantification.
3 Reagents and materials
Unless otherwise stated, the reagents used shall be the analytical reagent; the water shall
be the secondary deionized water.
3.1 Methanol. chromatographically pure reagent.
3.2 Methylisothiazolinone (2-methyl-4-isothiazolone-3-ketone). the purity is ≥ 98%.
3.3 Chloromethylisothiazolinone (5-chlorine-2-methyl-4-isothiazolone-3-ketone). the purity
is ≥ 98%.
3.4 Standard-stock mixed solution of methylisothiazolinone and
chloromethylisothiazolinone. accurately weigh (3.2) 0.025g of methylisothiazolinone and
(3.3) 0.1g of chloromethylisothiazolinone respectively. The accuracy is 0.0001 g. Place
them in the 50 mL beaker; add appropriate amount of methanol to dissolve it. Transfer
quantitative solution in to the 100mL volumetric flask; dilute it with methanol to the scale;
mix it uniformly. In this solution, the concentration of methylisothiazolinone is 250mg/L; the
concentration of chloromethylisothiazolinone is 1000mg/L. The stock solution shall be
stored in the refrigerator for cold storage.
5.2.2 Drawing of the standard working curve
Accurately and respectively absorb the standard working solution (3.5) for 10μL; inject
them into the liquid chromatograph in the order of the concentration from the dilute to the
concentrated; perform the determination according to the chromatographic condition
(5.2.1); use the peak area of the chromatographic peak as the ordinate AND use the
corresponding concentration as the abscissa to draw the diagram; draw the standard
working curve. The liquid chromatogram of the standard substance of
methylisothiazolinone and chloromethylisothiazolinone is shown in Appendix A.
5.2.3 Sample Determination
Use micro syringes to accurately absorb 10μL of sample solution (5.1); inject into the liquid
chromatograph; perform the determination according to the chromatographic condition
(5.2.1); record the retention time and peak area of the chromatographic peak. From the
peak area of the chromatographic peak, it can obtain the concentration of the
corresponding tested substance from the standard curve. In the sample solution, both of
the response value of methylisothiazolinone and chloromethylisothiazolinone shall be
within the linear range of instrumental determination. For the samples in which the content
of tested substance is high, it can take appropriate sample solution to perform
determination after diluting with methanol.
5.3 Blank test
In addition to not-weigh the sample, it shall be performed according to the above procedure.
6 Results calculation
The results shall be calculated as formula (1).
Where.
W - the content of methylisothiazolinone or chloromethylisothiazolinone in sample, %;
c - the concentration of methylisothiazolinone or chloromethylisothiazolinone in the
sample solution, which is obtained in the standard working curve. The unit is milligram
per liter (mg/L);
V - final constant volume of the sample solution. The unit is liter (L);
m - the mass of the sample. The unit is gram (g);
The calculation results shall be accurate to 0.001.
...... Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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