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
GB/T 35801-2018
GB
NATIONAL STANDARD OF THE
PEOPLE’S 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 0.45μm 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, 5μm, 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. 10μL.
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, 3.5μm, 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. 5μL.
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