GB/T 40744-2021 in English
VALIDDetermination of solanesol in potato stems,leaves and their processed products—High performance liquid chromatography-mass spectrometry
- Issued on:2021-10-11
- Implemented on:2022-05-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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《GB/T 40744-2021马铃薯茎叶及其加工制品中茄尼醇的含量测定 高效液相色谱-质谱法》由424-cnis（中国标准化研究院）归口，主管部门为国家市场监督管理总局。
Introduction
Technical Background of the Standard
This standard establishes for the first time a standardized method for the determination of solanesol in potato stem and leaf resources by high performance liquid chromatography-mass spectrometry. As an important pharmaceutical intermediate, the accurate determination of solanesol is of key significance for the high-value utilization of agricultural by-products.
Detailed explanation of the principle of the method
| Steps | Technical parameters | Mechanism of action |
|---|---|---|
| Extraction | n-hexane solvent, 45℃ ultrasonic for 30min | Dissolve free and esterified solanesol |
| Saponification | 0.02mol/L NaOH ethanol solution, 65℃ water bath for 2h | Release bound solanesol |
| Purification | Water washing, centrifugal stratification | Remove water-soluble impurities |
Key instrument configuration
Chromatographic conditions: A C18 column (150mm×2.1mm, 3.5μm) was used, the mobile phase was methanol-isopropanol (50:50), and the flow rate was 0.4mL/min.
Mass spectrometer parameters: ESI positive ion mode, monitoring m/z 653.6 characteristic ion, spray voltage 3500V, capillary temperature 350℃.
Method validation data
The method validation showed: detection limit 0.1mg/kg, quantification limit 0.3mg/kg, spike recovery 98%-101%, RSD<6.6%. The precision experiment showed that the intra-day RSD was ≤5.1% and the inter-day RSD was ≤4.8%.
Implementation recommendations
- The entire sample processing process must be kept away from light to prevent photolysis of solanesol
- The standard solution is recommended to be prepared and used immediately, and stored at 4°C away from light for no more than 3 months
- Quality control samples should be interspersed with each batch of testing to ensure instrument stability
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