GA/T 1620-2019 in English
VALIDForensic sciences—Examination methods for chlorpheniramine in biological samples—GC and GC-MS
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Introduction
Analysis of Standard Technical Framework
| Technical Dimension | Gas Chromatography (GC) | Gas Chromatography-Mass Spectrometry (GC-MS) |
|---|---|---|
| Detection Capability | Quantitative Analysis | Qualitative + Quantitative Analysis |
| Characteristic Indicators | Retention Time | Characteristic Ion Fragments (203/58/167) |
| Detection Limit | 0.1μg/mL(g) (Uniform Requirements) | |
| Recovery rate | Solid phase extraction (91.4%)>Liquid-liquid extraction (80.4%) | |
Core operation points
Comparison of sample pretreatment technologies
The standard stipulates two extraction methods: liquid-liquid extraction uses a methanol/acetonitrile (15:85) mixed solvent, which is simple to operate but has a low recovery rate; solid phase extraction uses a C18 column with ammonia/chloroform/isopropanol (2:78:20) elution. Although the steps are cumbersome, the recovery rate is increased by 11%.
Key Instrument Parameters
Gas chromatograph needs to be equipped with FID detector, DB-5 capillary column (30m×0.25mm×0.25μm) is recommended, column temperature program is 150℃(1min)→10℃/min→280℃(20min). GC-MS needs to meet the detection of characteristic ions 203 (base peak), 58, 167, ion source temperature 250℃.
Quality Control and Result Evaluation
The standard requires that parallel sample testing must be carried out, and the relative difference (RD) ≤20% is valid data. Qualitative judgment must meet the following requirements:
- Retention time deviation ±1%
- Detection of ≥3 characteristic ions
- Ion abundance ratio complies with the allowable deviation in Table 1
Implementation suggestions
Method optimization direction
For liver samples with complex matrices, it is recommended to:
- Increase the amount of phosphate buffer (pH10) to 8mL
- Extend the ultrasonic time to 20min
- Use matrix-matched standard curve for calibration
Standard evolution trend
Main improvements of the current standard compared with the earlier method:
- Introduction of solid phase extraction technology to improve recovery rate
- Clear criteria for determining characteristic ion abundance ratio
- Unify column temperature programs for GC and GC-MS

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