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GB/T 35801-2018 English PDF (GBT35801-2018)

GB/T 35801-2018 English PDF (GBT35801-2018)

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GB/T 35801-2018: Determination of prohibited captan in cosmetics -- High performance liquid chromatography

This Standard specifies determination method of high performance liquid chromatography for prohibited captan in cosmetics. This Standard is applicable to determination of captan in creams, liquids, loose powder cosmetics. The detection limit of this Standard for captan is 2 mg/kg, and the limit of quantification is 5 mg/kg.
GB/T 35801-2018
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.100.70
Y 42
Determination of prohibited captan in cosmetics -
High performance liquid chromatography
ISSUED ON. FEBRUARY 06, 2018
IMPLEMENTED ON. SEPTEMBER 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Normative references ... 5
3 Principle ... 5
4 Reagents and materials ... 5
5 Apparatus and equipment ... 6
6 Analysis steps ... 6
7 Result calculation ... 8
8 Detection limit and limit of quantification ... 8
9 Recovery rate and precision ... 8
10 Tolerance ... 8
Annex A (informative) Structural formula, high performance liquid
chromatogram and ultraviolet absorption spectrum of the captan standard product ... 9
Annex B (informative) Test of confirmation ... 11
Determination of prohibited captan in cosmetics -
High performance liquid chromatography
1 Scope
This Standard specifies determination method of high performance liquid chromatography for prohibited captan in cosmetics.
This Standard is applicable to determination of captan in creams, liquids, loose powder cosmetics.
The detection limit of this Standard for captan is 2 mg/kg, and the limit of quantification is 5 mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682, Water for analytical laboratory use - Specification and test methods
3 Principle
After the specimen is ultrasonically extracted by solvent and is centrifuged, use high performance liquid chromatography to determine, use external standard method to quantify, use liquid chromatography-mass spectrometry to confirm. 4 Reagents and materials
Unless otherwise stated, the reagents used are analytically pure, the water is of grade one specified in GB/T 6682.
4.1 Acetonitrile. chromatographically pure.
4.2 Methanol. chromatographically pure.
4.3 Tetrahydrofuran.
6.1.2 Liquid and loose powder samples
Weigh 1g (to the nearest of 0.001g) of sample. Place in a 10mL plugged plastic centrifuge tube (5.6). Shake well. Add into 10mL of methanol (4.2). After performing ultrasonic extraction for 20min, centrifugation at 5000r/min for 15min, the supernatant is filtered through a 0.45??m microporous membrane for
determination of high performance liquid chromatography.
6.2 Determination conditions
The reference conditions for high performance liquid chromatography are as follows.
a) Chromatographic column. C18, 5??m, 250mm ?? 4.6mm (inner diameter), or the equivalent;
b) Flow rate. 1.0mL/min;
c) Mobile phase. acetonitrile + water = 65 + 35 (volume ratio);
d) Detection wavelength. 206nm;
e) Column temperature. 30??C;
f) Injection volume. 10??L.
6.3 Drawing of standard curve
The captan standard working solution (4.7) was determined according to the determination conditions in 6.2 and the concentration from low to high injection. Draw in peak area-concentration. Make standard working curve.
See Figure A.2 in Annex A for a high performance liquid chromatogram of the captan standard solution. The UV absorption spectrum of the captan standard product is shown in Figure A.3 of Annex A.
6.4 Determination
Conduct determination for the testing sample according to the determination conditions in 6.2. If the retention time of the chromatographic peak detected is consistent with the standard product, and the chromatogram of the sample after subtracting the background, the UV absorption spectrum of the substance is consistent with the standard product, it can be preliminarily determined that captan exists in the sample. Use external standard method to quantify. The content of captan shall be within the standard curve. If it is outside the linear range, it shall be diluted before analysis. If necessary, positive sample shall be confirmed by liquid chromatography-mass spectrometry. See Annex B for
confirmation test.
Annex B
(informative)
Test of confirmation
B.1 Liquid chromatography conditions
The reference conditions for liquid chromatography determination are as follows.
a) Chromatographic column. XBridge C18, 3.5??m, 150mm ?? 2.1mm (inner
diameter);
b) Mobile phase. 0.1% formic acid solution + acetonitrile = 10 + 90 (volume ratio);
c) Flow rate. 0.3mL/min;
d) Column temperature. 30??C;
e) Injection volume. 5??L.
B.2 Mass spectrometry conditions
The reference conditions for mass spectrometry are as follows.
a) Ion source. electrospray ion source;
b) Ionization mode. positive ion mode;
c) Capillary voltage. 3.5kV;
d) Extraction voltage. 3.0V;
e) Ion source temperature. 150??C;
f) Desolvation gas temperature. 500??C;
g) Data collection method. multiple reaction monitoring.
B.3 Qualitative determination
When the specimen is measured, the sample solution is appropriately diluted, and the sample solution and the standard working solution are determined according to liquid chromatography-mass spectrometry conditions. If the selected ions are present, and the selected ion ratio is consistent with the

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