GA/T 1617-2019 in English
VALIDForensic sciences—Examination methods for brucine and strychnine in biological samples—HPLC and LC-MS
- Issued on:2019-10-14
- Implemented on:2019-12-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$214.00
Introduction
Analysis of Standard Technical Framework
| Technical Dimensions | HPLC Method | LC-MS Method |
|---|---|---|
| Detection Properties | Quantitative Analysis | Qualitative and Quantitative Analysis |
| Detection Limit | 20ng/g(mL) | 0.2ng/g(mL) |
| Characteristic Parameters | Retention Time + UV Spectrum | Ion Pair + Abundance Ratio |
Key Operation Points
Extraction process using Oasis® MCX SPE cartridge as an example:
- Centrifuge under acidic conditions to obtain the supernatant
- Load the SPE cartridge after activation (flow rate 1mL/min)
- Collect the alkaline eluate and concentrate it at 40℃
Quality Control System Construction
Standard requirements must include:
- Blank sample (matrix matching)
- Add recovery sample (concentration of 10ng/mL(g))
- Double parallel experiments (RD≤20%)
Methodology Validation Data
The LC-MS method uses the MRM mode of triple quadrupole mass spectrometry. The characteristic ion pairs of strychnine are:
| Quantitative ion | 395.20→324.10 |
| Qualifier ion | 395.20→224.20 |
Implementation Suggestions
Key Control Points:
1. pH adjustment must be accurate to 9.5±0.1 (ammonium acetate buffer system)
2. Attention should be paid to the following when optimizing mass spectrometry parameters:
- Capillary voltage 3.0kV
- Collision energy 30-35eV
3. The standard solution needs to be stored at -20℃ away from light and is valid for 6 months.
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