GB/T 33273-2016 English PDF (GB/T33273-2016)

GB/T 33273-2016: Textiles - Determination of triclosan residues
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GB/T 33273-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Textiles - Determination of triclosan residues
ISSUED ON: DECEMBER 13, 2016
IMPLEMENTED ON: JULY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents and materials ... 5 
5 Apparatus ... 5 
6 Sample pretreatment ... 6 
7 Determination ... 7 
8 Blank tests ... 13 
9 Calculation of results ... 13 
10 Lower detection limit and recovery rate ... 14 
11 Precision ... 14 
12 Test report... 14 
Appendix A (Informative) Typical chromatograms of triclosan and its derivative
... 15 
4 Reagents and materials
Unless otherwise stated, the reagents used in the analysis are of analytical
grade.
4.1 Water: The pretreatment water is the grade 3 water specified in GB/T 6682.
The water for analytical instrument is the grade 1 water specified in GB/T 6682.
4.2 Methanol: Chromatographically pure.
4.3 N-hexane: Chromatographically pure.
4.4 Acetic anhydride: Purity≥98.5%.
4.5 Sodium tetraborate solution, 0.1 mol/L: WEIGH 38.1 g of sodium tetraborate;
USE water to dissolve and dilute to 1000 mL.
4.6 Triclosan standard: CAS No. 3380-34-5. Purity>99.5%.
4.7 Standard stock solution: Accurately weigh an appropriate amount of
triclosan standard (4.6) to the nearest 0.1 mg; USE methanol (4.2) to prepare
a triclosan standard stock solution with a concentration of 100 mg/L.
4.8 Standard working solution: Accurately pipette an appropriate volume of
triclosan standard stock solution (4.7); USE methanol (4.2) to dilute to the
standard solution with required concentration.
Note: The standard stock solution is stored in the refrigerator at 0 °C~4 °C; the expiry date
is 6 months. The standard working solution is stored in the refrigerator at 0 °C~4 °C;
the expiry date is 3 months.
4.9 Organic-phase filter membrane: 0.45 μm filter membrane.
5 Apparatus
5.1 Analytical instruments: According to the selected method, select the
following instruments.
5.1.1 High-performance liquid chromatograph: Equipped with diode array
detector or ultraviolet detector.
5.1.2 Liquid chromatograph-tandem mass spectrometer: Equipped with
electrospray ionization source.
5.1.3 Gas chromatograph: Equipped with electron capture detector.
times. The upper organic phase is filtered through a filter membrane (4.9); and
then analyzed by gas chromatography (5.1.3), gas chromatography-mass
spectrometry (5.1.4), or gas chromatography-tandem mass spectrometry
(5.1.5). If necessary, perform instrument analysis after dilution.
7 Determination
7.1 High-performance liquid chromatography
7.1.1 Analysis conditions of high-performance liquid chromatography
Since the test results depend on the instrument used, it is impossible to give
general parameters for liquid chromatography analysis. The set parameters
shall ensure that, during chromatographic determination, the measured
component and other components can be effectively separated. The
parameters given below are proved to be feasible.
a) Chromatographic column: C18 reversed-phase chromatographic column;
250 mm (column length)×4.6 mm (inner diameter)×5 μm (particle size); or
equivalent;
b) Mobile phase: Methanol + water (90+10, volume ratio);
c) Flow rate: 1.0 mL/min;
d) Column temperature: 40 °C;
e) Detection wavelength: 282 nm;
f) Injection volume: 20.0 μL.
7.1.2 Standard working curve
According to 7.1.1, the standard working solution (4.8) is injected for
determination. USE the triclosan concentration as the abscissa and the peak
area as the ordinate, to draw the standard working curve. Under the above
liquid chromatography analysis conditions, the liquid chromatogram of the
triclosan standard solution is shown in Figure A.1 a) in Appendix A.
7.1.3 Qualitative and quantitative analysis
According to 7.1.1, the sample solution (6.2.1) is injected for determination.
According to the retention time of chromatographic peak, perform qualitative
analysis. When necessary, confirm in conjunction with ultraviolet absorption
spectrogram. Based on the peak area of the chromatographic peak, use the
external standard method for quantification.
f) Injection volume: 1.0 μL;
g) Injection method: Splitless injection.
7.3.2 Standard working curve
After the standard working solution (4.8) is derivatization pretreated according
to the method of 6.2.2, according to 7.3.1, it is injected for determination. USE
the triclosan concentration as the abscissa and the peak area as the ordinate,
to draw the standard working curve. Under the above conditions, the gas
chromatogram of the standard solution of triclosan derivative is shown in Figure
A.2 a) of Appendix A.
7.3.3 Qualitative and quantitative analysis
According to the analysis conditions of 7.3.1, the sample solution (6.2.2) is
injected for determination. According to the retention time of chromatographic
peak, perform qualitative analysis. When necessary, confirm in conjunction with
gas chromatography-mass spectrometry (7.4). Based on the peak area of the
chromatographic peak, use the external standard method for quantification.
7.4 Gas chromatography-mass spectrometry
7.4.1 Analysis conditions of gas chromatography-mass spectrometry
Since the test results depend on the instrument used, it is impossible to give
general parameters for gas chromatography-mass spectrometry analysis. The
set parameters shall ensure that, during chromatographic determination, the
measured component and other components can be effectively separated. The
parameters given below are proved to be feasible.
7.4.1.1 Analysis conditions of gas chromatography:
a) Chromatographic column: DB-5MS quartz capillary column; 30 m (column
length)×0.25 mm (inner diameter)×0.25 μm (film thickness); or equivalent;
b) Chromatographic column temperature: 150 °C 280 °C (3.5 min);
c) Inlet temperature: 280 °C;
d) Chromatograph-mass spectrometer interface temperature: 280 °C;
e) Carrier gas: Helium, purity≥99.999%. Flow rate is 1.0 mL/min;
f) Injection volume: 1.0 μL;
g) Injection method: Splitless injection. Open the valve after 1.0 min.
to draw the standard working curve. Under the above conditions, the gas
chromatography-tandem mass spectrometry chromatogram of the standard
solution of triclosan derivative is shown in Figure A.2 c) of Appendix A.
7.5.3 Qualitative and quantitative analysis
According to 7.5.1, the sample solution (6.2.2) is injected for determination.
According to the retention time of chromatographic peak, perform qualitative
analysis. Confirm in conjunction with the mass spectrogram. Based on the peak
area of the chromatographic peak, use the external standard method for
quantification.
8 Blank tests
Except that no sample is added, the determination steps of 6.1~7.5 above are
followed.
9 Calculation of results
According to formula (1), calculate the content of triclosan in textiles:
Where:
x - The content of triclosan in the sample, in milligrams per kilogram (mg/kg);
c - The concentration of triclosan read from the standard working curve of the
sample solution, in milligrams per liter (mg/L);
c0 - The concentration of triclosan read from the standard working curve in the
blank test, in milligrams per liter (mg/L);
V - The final constant volume of the sample, in milliliters (mL);
F - The dilution factor of the sample;
m - The mass of the sample, in grams (g).
The calculation result is shown to one decimal place. When below the lower
detection limit, the test result is not-detectable.
GB/T 33273-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Textiles - Determination of triclosan residues
ISSUED ON: DECEMBER 13, 2016
IMPLEMENTED ON: JULY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents and materials ... 5 
5 Apparatus ... 5 
6 Sample pretreatment ... 6 
7 Determination ... 7 
8 Blank tests ... 13 
9 Calculation of results ... 13 
10 Lower detection limit and recovery rate ... 14 
11 Precision ... 14 
12 Test report... 14 
Appendix A (Informative) Typical chromatograms of triclosan and its derivative
... 15 
4 Reagents and materials
Unless otherwise stated, the reagents used in the analysis are of analytical
grade.
4.1 Water: The pretreatment water is the grade 3 water specified in GB/T 6682.
The water for analytical instrument is the grade 1 water specified in GB/T 6682.
4.2 Methanol: Chromatographically pure.
4.3 N-hexane: Chromatographically pure.
4.4 Acetic anhydride: Purity≥98.5%.
4.5 Sodium tetraborate solution, 0.1 mol/L: WEIGH 38.1 g of sodium tetraborate;
USE water to dissolve and dilute to 1000 mL.
4.6 Triclosan standard: CAS No. 3380-34-5. Purity>99.5%.
4.7 Standard stock solution: Accurately weigh an appropriate amount of
triclosan standard (4.6) to the nearest 0.1 mg; USE methanol (4.2) to prepare
a triclosan standard stock solution with a concentration of 100 mg/L.
4.8 Standard working solution: Accurately pipette an appropriate volume of
triclosan standard stock solution (4.7); USE methanol (4.2) to dilute to the
standard solution with required concentration.
Note: The standard stock solution is stored in the refrigerator at 0 °C~4 °C; the expiry date
is 6 months. The standard working solution is stored in the refrigerator at 0 °C~4 °C;
the expiry date is 3 months.
4.9 Organic-phase filter membrane: 0.45 μm filter membrane.
5 Apparatus
5.1 Analytical instruments: According to the selected method, select the
following instruments.
5.1.1 High-performance liquid chromatograph: Equipped with diode array
detector or ultraviolet detector.
5.1.2 Liquid chromatograph-tandem mass spectrometer: Equipped with
electrospray ionization source.
5.1.3 Gas chromatograph: Equipped with electron capture detector.
times. The upper organic phase is filtered through a filter membrane (4.9); and
then analyzed by gas chromatography (5.1.3), gas chromatography-mass
spectrometry (5.1.4), or gas chromatography-tandem mass spectrometry
(5.1.5). If necessary, perform instrument analysis after dilution.
7 Determination
7.1 High-performance liquid chromatography
7.1.1 Analysis conditions of high-performance liquid chromatography
Since the test results depend on the instrument used, it is impossible to give
general parameters for liquid chromatography analysis. The set parameters
shall ensure that, during chromatographic determination, the measured
component and other components can be effectively separated. The
parameters given below are proved to be feasible.
a) Chromatographic column: C18 reversed-phase chromatographic column;
250 mm (column length)×4.6 mm (inner diameter)×5 μm (particle size); or
equivalent;
b) Mobile phase: Methanol + water (90+10, volume ratio);
c) Flow rate: 1.0 mL/min;
d) Column temperature: 40 °C;
e) Detection wavelength: 282 nm;
f) Injection volume: 20.0 μL.
7.1.2 Standard working curve
According to 7.1.1, the standard working solution (4.8) is injected for
determination. USE the triclosan concentration as the abscissa and the peak
area as the ordinate, to draw the standard working curve. Under the above
liquid chromatography analysis conditions, the liquid chromatogram of the
triclosan standard solution is shown in Figure A.1 a) in Appendix A.
7.1.3 Qualitative and quantitative analysis
According to 7.1.1, the sample solution (6.2.1) is injected for determination.
According to the retention time of chromatographic peak, perform qualitative
analysis. When necessary, confirm in conjunction with ultraviolet absorption
spectrogram. Based on the peak area of the chromatographic peak, use the
external standard method for quantification.
f) Injection volume: 1.0 μL;
g) Injection method: Splitless injection.
7.3.2 Standard working curve
After the standard working solution (4.8) is derivatization pretreated according
to the method of 6.2.2, according to 7.3.1, it is injected for determination. USE
the triclosan concentration as the abscissa and the peak area as the ordinate,
to draw the standard working curve. Under the above conditions, the gas
chromatogram of the standard solution of triclosan derivative is shown in Figure
A.2 a) of Appendix A.
7.3.3 Qualitative and quantitative analysis
According to the analysis conditions of 7.3.1, the sample solution (6.2.2) is
injected for determination. According to the retention time of chromatographic
peak, perform qualitative analysis. When necessary, confirm in conjunction with
gas chromatography-mass spectrometry (7.4). Based on the peak area of the
chromatographic peak, use the external standard method for quantification.
7.4 Gas chromatography-mass spectrometry
7.4.1 Analysis conditions of gas chromatography-mass spectrometry
Since the test results depend on the instrument used, it is impossible to give
general parameters for gas chromatography-mass spectrometry analysis. The
set parameters shall ensure that, during chromatographic determination, the
measured component and other components can be effectively separated. The
parameters given below are proved to be feasible.
7.4.1.1 Analysis conditions of gas chromatography:
a) Chromatographic column: DB-5MS quartz capillary column; 30 m (column
length)×0.25 mm (inner diameter)×0.25 μm (film thickness); or equivalent;
b) Chromatographic column temperature: 150 °C 280 °C (3.5 min);
c) Inlet temperature: 280 °C;
d) Chromatograph-mass spectrometer interface temperature: 280 °C;
e) Carrier gas: Helium, purity≥99.999%. Flow rate is 1.0 mL/min;
f...