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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China National Textile and Apparel Council.
This standard is under the jurisdiction of the National Technical Committee on Textiles of Standardization Administration of China (SAC/TC 209).
Textiles - Determination of triclosan residues
Warning: the personnel using this standard shall be experienced in regular laboratory work. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies five methods for determination of triclosan residues in textiles, i.e., high-performance liquid chromatography, liquid chromatography-tandem mass spectrometry, gas chromatography, gas chromatography-mass spectrometry and gas chromatography-tandem mass spectrometry.
This standard is applicable to textile materials and their products.
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
Non-derivatization pretreatment method: the specimen is ultrasonically extracted with methanol, and after the extract is concentrated to constant volume, the triclosan residues in textiles are determined by high-performance liquid chromatography or liquid chromatography-tandem mass spectrometry, and quantified by external standard method.
Derivatization pretreatment method: the specimen is ultrasonically extracted with methanol, the extract is concentrated, transferred into sodium tetraborate solution, acetylated with acetic anhydride, and extracted with n-hexane; the triclosan residues in textiles are determined by gas chromatography, gas chromatography-mass spectrometry or gas chromatography-tandem mass spectrometry, and quantified by external standard method.
4 Reagents and materials
Unless otherwise specified, analytically-pure reagents shall be used in the analysis.
4.1 Water: Grade 3 water and Grade 1 water specified in GB/T 6682 are used for the pretreatment and the analytical instrument respectively.
4.2 Methanol: chromatographically pure.
4.3 n-hexane: chromatographically pure.
4.4 Acetic anhydride: with purity ≥ 98.5%.
4.5 Sodium tetraborate solution, 0.1mol/L: weigh 38.1g sodium tetraborate, dissolve in water and dilute to 1,000mL.
4.6 Triclosan: with CAS No. of 3380-34-5 and purity greater than 99.5%.
4.7 Standard stock solution: accurately weigh (accurate to 0.1mg) an appropriate amount of triclosan (4.6), and prepare a triclosan standard stock solution with a concentration of 100mg/L with methanol (4.2).
4.8 Standard working solution: accurately transfer an appropriate volume of triclosan standard stock solution (4.7), and dilute to standard solution with the required concentration with methanol (4.2).
Note: the standard stock solution is valid for six months stored in the refrigerator at 0℃~4℃; the standard working solution is valid for three months stored in the refrigerator at 0℃～4℃.
4.9 Organic phase filter membrane: 0.45μm.
5 Instruments
5.1 Analytical instruments: select the following instruments according to the method selected.
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.
5.1.4 Gas chromatograph-mass spectrometer: equipped with electron impact ionization source.
5.1.5 Gas chromatograph-tandem mass spectrometer: equipped with electron impact ionization source.
5.2 Vacuum rotary evaporator.
5.3 Temperature-controllable ultrasonic generator: with working frequency of 40kHz.
5.4 Oscillator: with oscillation frequency of 150 times/min.
5.5 Nitrogen blower.
5.6 Balance: with sensitivity of 0.01g and 0.1mg.
6 Specimen pretreatment
6.1 Specimen preparation and extraction
Take a representative sample and cut it into 5mm×5mm pieces, then mix them well. Weigh (accurate to 0.01g) about 1g specimen from the mixed sample, place it in a 150mL conical flask with plug, add 25mL methanol (4.2), perform ultrasonic extraction at 40℃ for 30min, and collect the extract into a round-bottom flask. Ultrasonically extract the residue with 25mL methanol (4.2) for 30min, and combine the extracts. At 40℃, concentrate the extract in the round-bottom flask to nearly 1mL with a rotary evaporator (5.2), and then slowly blow to nearly dry with nitrogen.
6.2 Extract treatment methods
6.2.1 Non-derivatization method: dissolve the residue (6.1) in the round-bottom flask with methanol to a constant volume of 10mL. Perform analysis using high-performance liquid chromatography (5.1.1) or liquid chromatography-tandem mass spectrometry (5.1.2) after filtering the solution by a filter membrane (4.9). Dilute if necessary and then perform instrument analysis.
6.2.2 Derivatization method: wash the residue (6.1) in the round-bottom flask for several times with 50mL sodium tetraborate solution (4.5), and transfer the washing liquid into a 150mL conical flask with plug. Add 1mL acetic anhydride (4.4) and oscillate with an oscillator (5.4) at 150 times/min for 30min at room temperature. Accurately add 10mL n-hexane (4.3) and continue oscillating for 30min. Transfer into a 125mL separating funnel, shake it well and keep it still, and discard the lower aqueous phase. Wash the upper organic phase with 30mL sodium tetraborate solution (4.5), shake it well and keep it still, discard the lower aqueous phase, and repeat washing for three times. Perform analysis using gas chromatography (5.1.3), gas chromatography-mass spectrometry (5.1.4) or gas chromatography-tandem mass spectrometry (5.1.5) after filtering the upper organic phase by a filter membrane (4.9). Dilute if necessary and then perform instrument analysis.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Instruments
6 Specimen pretreatment
7 Determination
8 Blank test
9 Result calculation
10 Lower detection limit and recovery rate
11 Precision
12 Test report
Annex A (Informative) Typical chromatograms of triclosan and its derivative
