摘要
目的建立l-OTS的含量测定及光学纯度检查的超高效合相色谱法(UPC^2)。方法使用ACQUITY UPC^(2TM)Trefoil^(TM)AMY1手性色谱柱(3.0 mm×50 mm,2.5μm),柱温30℃,以超临界CO_2和0.2%二乙胺的异丙醇(95∶5,体积比)为流动相,流速为1.0 m L/min,检测波长227 nm(补偿参比为310~360 nm),采用对照品法进行定量测定。结果 l-OTS与其对映异构体(d-OTS)有效分离,分离度为2.30,在40~1 000 mg/L范围内峰面积对应质量浓度呈良好的线性关系(r=0.999 9,n=7),平均加样回收率为99.8%(n=9),样品在24 h内稳定(RSD=0.81%),最低检测限5 ng(S/N=4)。结论此方法简便、迅速,经方法学验证可用于l-OTS的含量测定及光学纯度分析。
Objective To develop an ultra performance convergence chromatography（UPC） method for determining l-OTS level and optical purity.Methods Reference substance method was used for quantitative determination.The separation of enantiomers was achieved on a chiral chromatographic column ACQUITY UPC2TM TrefoilTM AMY1（3.0 mm×50 mm,2.5 mm） at the column temperature of 30℃ with the mobile phase of supercritical carbon dioxide-0.2%DEA in 2-propanol（95：5） at a flow rate of 1.0 mL/min.Detection wavelength was set at 227 nm（compensation reference was 310-360 nm）.Results l-OTS and its enantiomer（d-OTS） were effectively separated with the resolution of 2.30.Peak area was linear to mass concentration within the concentration rang of 40- 1 000 mg/L（r = 0.999 9,n=7）.Average recovery was 99.8%（n = 9）and the sample was stable within 24 h（RSD =0.81%）.The LOD was 5 ng（S/N =4）.Conclusion This method is simple and quick and can be used for determining l-OTS level and analyzing optical purity,which has been validated by methodology.
出处
《上海交通大学学报（医学版）》
CAS
CSCD
北大核心
2016年第3期459-462,共4页
Journal of Shanghai Jiao tong University:Medical Science
基金
高校教师专业发展计划(BJ13100150032)
国家自然科学基金(81171245)~~
关键词
超高效合相色谱法
莨菪烷衍生物
手性分析
光学纯度
ultra performance convergence chromatography
tropane derivatives
chiral separation
optical purity
