GB/T 39875-2021Examination methods for chlordiazepoxide in suspected drugs—Gas chromatography and gas chromatography-mass spectrometry (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This standard specifies the gas chromatography-mass spectrometry (GC-MS) qualitative inspection method and the gas chromatography (GC) quantitative inspection method of chlordiazepoxide.

Management, reagents and materials, instruments and equipment, operating methods, and result evaluation and presentation.

This standard applies to the qualitative and quantitative analysis of chlordiazepoxide in solid samples of suspected drugs.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 27418 Evaluation and Expression of Uncertainty in Measurement

GA/T 122 Terminology for toxicological analysis

3 Terms and definitions

The terms and definitions defined in GA/T 122 are applicable to this document.

4 Principle

Extract chlordiazepoxide in solid samples of suspected drugs. Detect by gas chromatography-mass spectrometry, with retention time and characteristic ion fragments And ion abundance ratio is used as the basis for qualitative judgment; gas chromatographic detection is used, and the chromatographic peak area is used as the quantitative basis, and the external standard single-point method or internal standard method is used as the quantitative basis. Standard curve method for quantitative analysis.

5 Reagents

Unless otherwise specified, the reagents used in the analysis are chromatographically pure.

5.2 Internal standard. Propyl spasmolytic (SKF525A) (purity not less than 95%).

5.3 Standard substance stock solution. 1.0mg/mL chlordiazepoxide standard substance stock solution, stored at 0°C~4°C, valid for 12 months.

5.4 Internal standard stock solution for quantitative internal standard curve method. Weigh 500 mg of SKF525A, dilute it with methanol to a 50 mL volumetric flask, and prepare it 10.0mg/mL SKF525A internal standard stock solution. Keep refrigerated at 0°C~4°C, valid for 12 months.

5.5 Standard working solution for qualitative use. Pipette an appropriate amount of chlordiazepoxide standard substance stock solution, dilute with methanol, and prepare 0.1mg/mL chlorazide Zhuo standard working solution. Store at 0°C~4°C, the validity period is 3 months.

5.6 Qualitative control standard working solution. Pipette an appropriate amount of chlordiazepoxide standard substance stock solution, dilute with methanol, and prepare a 0.005mg/mL solution.

5.7 Standard working solution for external standard single-point method quantification. pipette an appropriate amount of chlordiazepoxide standard substance stock solution, dilute with methanol, and prepare 0.1mg/mL The standard working solution of chlordiazepoxide. Store at 0°C~4°C, the validity period is 3 months.