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GB/T 45367-2025 PDF English

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GB/T 45367-2025: Textiles - Determination of camphor derivates
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GB/T 45367-2025: Textiles - Determination of camphor derivates

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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 59.080.01 CCS W 04 Textiles - Determination of camphor derivates Issued on: FEBRUARY 28, 2025 Implemented on: SEPTEMBER 01, 2025 Issued by. State Administration for Market Regulation; Standardization Administration of the People's Republic of China.

Table of Contents

Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Terms and definitions... 4 4 Principle... 4 5 Reagents and materials... 5 6 Instruments and equipment... 5 7 Analysis steps... 6 8 Result calculation and presentation... 7 9 Limit of quantitation and precision... 7 10 Test report... 8 Annex A (informative) LC-MS/MS analysis conditions... 9 Textiles - Determination of camphor derivates WARNING -- The personnel who use this document should have practical experience in formal laboratory work. This document does not point out all possible safety issues. The user is responsible for taking appropriate safety and health measures and ensuring that the conditions stipulated by relevant national laws and regulations are met.

1 Scope

This document describes a test method for the determination of camphor derivatives (3- benzylidene camphor and 4-methylbenzylidene camphor) in textiles using liquid chromatography-tandem mass spectrometry (LC-MS/MS). This document applies to all types of textile 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 GB/T 8170, Rules of rounding off for numerical values and expression and judgement of limiting values

3 Terms and definitions

There are no terms or definitions that require definition in this document.

4 Principle

The specimen is extracted with methanol by ultrasonic method. The extract is filtered through a filter membrane and then determined by LC-MS/MS. The external standard method is used for quantification.

5 Reagents and materials

Unless otherwise stated, all reagents used are analytically pure. 5.1 Water. Meet the requirements of Grade one water in GB/T 6682. 5.2 Methanol. CAS No. 67-56-1; chromatographically pure. 5.3 Ammonium formate. CAS No. 540-69-2; purity is not less than 99.0% (mass fraction). 5.4 Ammonium formate solution. 0.01 mol/L. Weigh 0.64 g of ammonium formate (5.3). Dissolve in water (5.1) and dilute to 1000 mL. Shake well. 5.5 3-Benzalkonium camphor standard substance/standard sample. CAS No. 15087-24- 8; purity is not less than 98.1% (mass fraction). 5.6 4-Methylbenzalkonium camphor standard substance/standard sample. CAS No. 36861-47-9; purity is not less than 98.1% (mass fraction). 5.7 Standard stock solution. The mass concentration is not less than 200 mg/L. Accurately weigh 3-benzylidene camphor standard substance/standard sample (5.5) and 4-methylbenzylidene camphor standard substance/standard sample (5.6). Prepare with methanol (5.2). NOTE. This solution should be stored in a refrigerator at 0℃~4℃ away from light. The validity period is 6 months. 5.8 Standard working solution. The mass concentration is 0.02 mg/L~0.5 mg/L. Accurately pipette an appropriate amount of standard stock solution (5.7). Dilute with methanol (5.2) to prepare. NOTE. This solution should be stored in a refrigerator at 0℃~4℃ away from light. The validity period is 3 months.

6 Instruments and equipment

6.1 Liquid chromatography-tandem mass spectrometer (LC-MS/MS). equipped with electrospray ionization source (ESI). 6.2 Analytical balance. graduation values are 0.01 g and 0.0001 g respectively. 6.3 Extractor. sealed with stopper; about 50 mL; made of hard glass. 6.4 Ultrasonic generator. working frequency is (40±5) kHz; temperature can be controlled to (50±2)℃. 6.5 Organic phase needle filter. polytetrafluoroethylene; pore size is 0.22 μm.

7 Analysis steps

7.1 Specimen preparation Select representative specimens. Cut into pieces of approximately 5 mm × 5 mm. Mix well. 7.2 Extraction Use an analytical balance (6.2) to weigh about 1.0 g of specimen (accurate to 0.01 g) and place in an extractor (6.3). Add 50.0 mL of methanol (5.2) accurately. Seal the extractor. Extract for (30±2) min in an ultrasonic generator (6.4) at (50±2)℃. Cool to room temperature within 2 min. Filter the specimen solution through an organic phase needle filter (6.5). Use LC-MS/MS (6.1) to analyze. 7.3 LC-MS/MS determination 7.3.1 Qualitative analysis Under the same test conditions, take equal volumes of the specimen solution (7.2) and the standard working solution (5.8). Inject them for determination. Test and analyze according to the conditions of 7.3.Qualitative analysis is performed by comparing the retention time and relative abundance of characteristic ions of the target in the specimen solution and the standard working solution. The deviation between the retention time of the target in the specimen and the retention time of the target in the standard working solution is within the range of ±2.5%. The relative abundance of the characteristic ions of the target in the sample is consistent with the relative abundance of the target in the standard working solution. If the relative abundance allowable deviation does not exceed the range specified in Table 1, it can be judged that the corresponding analyte exists in the sample. Annex A gives examples of LC-MS/MS analysis conditions. 7.3.2 Quantitative analysis Select at least 5 standard working solutions (5.8) of different mass concentrations for determination. Draw a standard curve with the peak area of the target substance versus ......

Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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