刑事技术Issue(3)：204-207,4.DOI:10.16467/j.1008-3650.2015.03.008
超高效液相色谱检测黄樟素方法研究
Determination of Safrole by Ultra Performance Liquid Chromatography
摘要
Abstract
ABSTRACT:To establish a quantitative method for determination of safrole by ultra performance liquid chromatography (UPLC), safrole samples were diluted by methanol, oscillated with the speed of 1500r/min for 10 minutes or ultrasound-assisted oscillated for 3 minutes, then ifltered the solution with 0.22 µm membrane and drew 1.5 mL for automatic injection. The separation was optimized and performed on a Shimadzu ODS-SP column (250 mm×4.6 mm, 5 µm). The mobile phase was pure water (A)-acetonitrile (B) and the mode of elution was gradient. The initial condition was 60%B, and the gradient steepness of organic phase was 0.5%/min between 0~13 min, then the organic phase’s content was raised to 95% immediately and held on for 7 minutes. The complete gradient elution procedure was 60%B (0.01 min)~66.5% B (13 min)~95%B (13.01 min)~95% B (20 min). Flow rate was set as 1 mL/min, column temperature was set as 40℃ and injection volume was set as 5 μL. The primary quantitative wavelength of UV detector was set as 210 nm and the auxiliary one was set as 235 nm. When the organic phase’s initial content increased, theoretical plate number and retention time decreased, but peak height increased. When the gradient steepness increased, theoretical plate number and peak height increased, but retention time decreased. Using the optimized method, good linearity was achieved over the range of 2~200 μg/mL. External standard working curve Y=1833.39X+5675.32, r2>0.9999. Limit of detection was 0.1 μg/mL under the condition of S/N>3. The precision was good with the intra-day RSDs less than 1.26% and inter-day RSDs less than 2.08%. The accuracy was also satisifed. The recovery rates were in the range of 98.21% to 102.18%, with RSDs between 0.35% and 0.96%. The test samples showed good stability under room temperature, freeze condition and three cycles of freeze-thaw condition. The RSDs of peak area of 6 samples placed at room temperature for 3, 6, 12, 24, 48, 96 hours were between 0.35% and 1.02%. The RSDs of 3 samples placed in refrigerator at -20℃ for 5, 10, 15 days were between 0.58% and 1.67%. The RSDs of 3 samples which were frozen and thawed three times were between 0.26% and 0.93%. The method was proved to be good when applied to case samples. For example, once we received an unknown sample seized by police, and then used the extraction and chromatography methods to analyze the sample, the major analyte’s retention time was consistent with safrole standard and the quantitative result was 7.08%. This method was rapid, simple, effective and suited for quantitative determination of safrole.关键词
超高效液相色谱/黄樟素/定量分析Key words
ultra performance liquid chromatography/safrole/quantitative analysis分类
社会科学引用本文复制引用
翟晚枫,李彭,贺剑锋,高利生..超高效液相色谱检测黄樟素方法研究[J].刑事技术,2015,(3):204-207,4.基金项目
中央级公益性科研院所基本科研业务费项目 （）
