GB/T 40641-2021 in English
VALIDDetermination of polyprenol from pine needles—High performance liquid chromatography
- Issued on:2021-10-11
- Implemented on:2022-05-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$97.00
《GB/T 40641-2021松针聚戊烯醇含量的测定 高效液相色谱法》由TC558（全国林化产品标准化技术委员会）归口，主管部门为国家林业和草原局。
Introduction
Technical background and significance of the standard
This standard was proposed by the State Forestry and Grassland Administration and managed by the National Forestry Products Standardization Technical Committee, filling the gap in the standard for the detection of active ingredients in pine needles. As a high-value-added component in pine needle extracts, the accurate quantification of polyprenols is of great significance to the development of forestry resources and the quality control of health products.
Analysis of core detection methods
| Key steps | Technical parameters | Quality control points |
|---|---|---|
| Sample extraction | Petroleum ether refluxed at 65℃ for 2h | Water content ≤3% |
| Purification process | Silica gel column chromatography gradient elution | Sample amount: silica gel = 1:3 |
| Chromatographic conditions | C18 column (150mm×4.6mm) | Detection wavelength 210nm |
Instrument configuration requirements
The main equipment includes: High performance liquid chromatograph (with UV detector), Rotary evaporator, Vacuum drying oven, etc. The chromatographic column must meet the specifications of C18 reverse phase column, with a particle size of 5μm and a column temperature control accuracy of ±0.5℃.
Method validation data
The standard stipulates that the limit of quantification is 4μg/kg, and the precision requires that the absolute difference between two parallel determinations is ≤5%. A standard curve is established through 6 concentration gradients (0.10-6.00mg/mL), with C65-C85 as the main characteristic peaks for calculation.
Implementation suggestions
Common problem handling
1. When the sample peak is higher than 6.00mg/mL, the concentration range of the standard curve needs to be expanded
2. The saponification process needs to strictly control the 80℃ water bath temperature and time (3.5h±5min)
3. Storage conditions of standard substances: refrigerated below 4℃ and valid for 2 months
Method optimization direction
Ultrasound-assisted extraction technology can be explored to shorten the pre-treatment time, or LC-MS coupling technology can be used to improve qualitative accuracy.
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