Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This Standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of the National Technical Committee 272 on Surfactant Soap and Detergent of Standardization Administration of China (SAC/TC272).
Cleaning products - Determination of triclosan
1 Scope
This standard specifies the method for determination of triclosan in cleaning products by high performance liquid chromatography.
This standard is applicable to determination of triclosan in cleaning products.
2 Normative references
The following documents are essential for the application of this Standard. For the dated normative references, only the dated editions are applicable to this document. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Principle
The specimen is dissolved by mobile phase and then extracted by ultrasonic wave; the filtered extract is tested by high performance liquid chromatograph equipped with UV detector or diode-array detector. The specimen is determined qualitatively by the retention time of the component under test, and quantitatively by external standard methods.
4 Reagents and materials
Unless otherwise specified, analytic pure reagents and Class-2 water conforming to GB/T 6682 shall be used in the tests.
4.1 Methanol: chromatographically pure.
4.2 Triclosan (CAS: 3380-34-5; molecular formula: C12H7Cl3O2): with a purity of greater than or equal to 99%.
4.3 Triclosan stock solution: accurately weigh 100mg of triclosan (4.2), dissolve it with methanol to 100mL, preparing it into a stock solution with a concentration of 1000 mg/L; preserve it in a 4℃refrigerator; prepare the standard solutions with appropriate concentrations as required and plot the standard curves.
4.4 Filter membrane: organic, 0.45 μm.
5 Apparatus
5.1 High performance liquid chromatograph: equipped with diode array or UV detector.
5.2 Analytical balance: with a sensitivity of 0.1mg.
5.3 Ultrasonic cleaner.
5.4 Centrifuge: with a rotation speed of not less than 4000 r/min.
6 Determination
6.1 Specimen preparation
Weigh 0.5g of the sample in a liquid or paste condition (0.2g of solid sample) (accurate to 1mg), place it in a 25mL of volumetric flask, add 15mL of mobile phase; perform ultrasonic extraction for 20min; dilute it with mobile phase to the scale and mix well. If the solution is turbid, shift the extract with the constant volume to a centrifuge tube, centrifugalize it at 4000r/min for 10min; filter the supernatant liquor with filter membrane (4.4); conduct determination on the obtained filtrate by high performance liquid chromatography.
6.2 Determination with high performance liquid chromatography
6.2.1 Chromatography reference condition
Chromatography reference conditions are as follows:
a) Chromatographic column: C18 siloxane-bonded silica column with 5μm fillers and dimensions of 250mm × 4.6mm (inner diameter), or chromatographic column with equivalent performance;
Note: as C18 chromatographic columns with different batch number or STD have different retention time to triclosan component, the proportion of methanol and water in the mobile phase may be adjusted to ensure the suitable elution time of the sample.
b) Mobile phase: methanol + water (77 + 23, in mass ratio);
c) Flow rate: 1.0 mL/min;
d) Detection wavelength: 281 nm;
e) Sample injection: 10 μl or equivalent injection;
f) Column temperature: ambient temperature.
6.2.2 Plotting of standard curve
Pipette triclosan stock solution (4.3) to prepare the working solutions with concentrations of 1.0 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L and 50.0 mg/L. Conduct the determination in the chromatographic conditions (6.2.1); with the peak area as longitudinal coordinate and triclosan working solution concentration as horizontal coordinate, plot the standard curve; determine qualitatively by the retention time, and quantitatively by external standard method. The chromatograph chart of triclosan in the conditions (6.2.1) is shown in Figure A.1, Annex A hereto.
Foreword i 1 Scope 2 Normative references 3 Principle 4 Reagents and materials 5 Apparatus 6 Determination 7 Recovery factor and limit of quantification 8 Precision Annex A (Informative) Chromatograph chart of triclosan standard substance
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This Standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of the National Technical Committee 272 on Surfactant Soap and Detergent of Standardization Administration of China (SAC/TC272).
Cleaning products - Determination of triclosan
1 Scope
This standard specifies the method for determination of triclosan in cleaning products by high performance liquid chromatography.
This standard is applicable to determination of triclosan in cleaning products.
2 Normative references
The following documents are essential for the application of this Standard. For the dated normative references, only the dated editions are applicable to this document. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Principle
The specimen is dissolved by mobile phase and then extracted by ultrasonic wave; the filtered extract is tested by high performance liquid chromatograph equipped with UV detector or diode-array detector. The specimen is determined qualitatively by the retention time of the component under test, and quantitatively by external standard methods.
4 Reagents and materials
Unless otherwise specified, analytic pure reagents and Class-2 water conforming to GB/T 6682 shall be used in the tests.
4.1 Methanol: chromatographically pure.
4.2 Triclosan (CAS: 3380-34-5; molecular formula: C12H7Cl3O2): with a purity of greater than or equal to 99%.
4.3 Triclosan stock solution: accurately weigh 100mg of triclosan (4.2), dissolve it with methanol to 100mL, preparing it into a stock solution with a concentration of 1000 mg/L; preserve it in a 4℃refrigerator; prepare the standard solutions with appropriate concentrations as required and plot the standard curves.
4.4 Filter membrane: organic, 0.45 μm.
5 Apparatus
5.1 High performance liquid chromatograph: equipped with diode array or UV detector.
5.2 Analytical balance: with a sensitivity of 0.1mg.
5.3 Ultrasonic cleaner.
5.4 Centrifuge: with a rotation speed of not less than 4000 r/min.
6 Determination
6.1 Specimen preparation
Weigh 0.5g of the sample in a liquid or paste condition (0.2g of solid sample) (accurate to 1mg), place it in a 25mL of volumetric flask, add 15mL of mobile phase; perform ultrasonic extraction for 20min; dilute it with mobile phase to the scale and mix well. If the solution is turbid, shift the extract with the constant volume to a centrifuge tube, centrifugalize it at 4000r/min for 10min; filter the supernatant liquor with filter membrane (4.4); conduct determination on the obtained filtrate by high performance liquid chromatography.
6.2 Determination with high performance liquid chromatography
6.2.1 Chromatography reference condition
Chromatography reference conditions are as follows:
a) Chromatographic column: C18 siloxane-bonded silica column with 5μm fillers and dimensions of 250mm × 4.6mm (inner diameter), or chromatographic column with equivalent performance;
Note: as C18 chromatographic columns with different batch number or STD have different retention time to triclosan component, the proportion of methanol and water in the mobile phase may be adjusted to ensure the suitable elution time of the sample.
b) Mobile phase: methanol + water (77 + 23, in mass ratio);
c) Flow rate: 1.0 mL/min;
d) Detection wavelength: 281 nm;
e) Sample injection: 10 μl or equivalent injection;
f) Column temperature: ambient temperature.
6.2.2 Plotting of standard curve
Pipette triclosan stock solution (4.3) to prepare the working solutions with concentrations of 1.0 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L and 50.0 mg/L. Conduct the determination in the chromatographic conditions (6.2.1); with the peak area as longitudinal coordinate and triclosan working solution concentration as horizontal coordinate, plot the standard curve; determine qualitatively by the retention time, and quantitatively by external standard method. The chromatograph chart of triclosan in the conditions (6.2.1) is shown in Figure A.1, Annex A hereto.
Contents of GB/T 35830-2018
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Apparatus
6 Determination
7 Recovery factor and limit of quantification
8 Precision
Annex A (Informative) Chromatograph chart of triclosan standard substance
