GA/T 1909-2021 in English
VALIDForensic sciences-Examination methods for a-solanine and a-chaconine in biological samples-LC-MS
- Issued on:2021-10-14
- Implemented on:2022-05-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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Introduction
Analysis of the Standard Technical Framework
| Core Elements | Technical Parameters | Innovation Points |
|---|---|---|
| Detection Objects | α-Solanine/α-Chaconine (Main Component of Solanine) | The First Establishment of a Forensic Science-Specific Detection Standard |
| Detection Limit | Blood/Urine 0.2ng/mL, Liver Tissue 0.2ng/g | Sensitivity 10 Times Higher Than Conventional HPLC Methods |
| Chromatographic Conditions | Restek Allure® PFP Propyl column (100mm×2.1mm, 5μm) | Special stationary phase improves the separation of glycoalkaloids |
Key operating points
Pretreatment optimization:Oasis® HLB solid phase extraction column was used, and the recovery rate was stable at 50-80% (see Table B.3), which was significantly better than the traditional liquid-liquid extraction method. Tissue samples need to add 0.2mL of water to compensate for the matrix effect.
Mass spectrometry parameters:In ESI+ mode, m/z 868.6/398.5 (α-solanine) and 852.6/706.5 (α-chaconine) were selected as quantitative ion pairs, and the collision energy was optimized to 93eV and 56eV (Appendix B Table B.1).
Method Validation Data
| Validation Indicators | Blood | Urine | Liver Tissue |
|---|---|---|---|
| Linear Range | 0.5-100ng/mL(g)（r＞0.997） | ||
| Intra-Day Precision | 2.49-10.07% | 3.98-8.23% | 2.64-10.65% |
| Matrix Effect | 45.8-66.4% | 52.5-79.7% | 45.0-66.1% |
Implementation suggestions
1. Quality control requirements:Blank samples and added sample controls must be performed simultaneously. If the relative difference (RD) exceeds 20%, retesting is required (Clause 8.2)
2. Result interpretation:A positive judgment must simultaneously meet the requirements of retention time deviation <±2.5%, two pairs of qualitative ion pairs matching, and abundance ratio error meeting the requirements of Table 2 (Clause 8.1.1)
3. Special circumstances: For corrupt samples, it is recommended to increase the activation volume of the solid phase extraction column to 2mL methanol/2mL water to prevent column efficiency from decreasing
Technology Evolution Analysis
Compared with the traditional colorimetric method, this standard: ① The detection limit is reduced by 2 orders of magnitude (from μg level to ng level); ② For the first time, the quantification of α-solanine and α-chaconine is achieved separately; ③ Primobolan acetate is introduced as an internal standard to effectively overcome the matrix effect (Appendix B Table B.3).
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