上海交通大学学报（医学版）

上海交通大学学报（医学版）

• 技术与方法 • 上一篇    

超高效合相色谱法测定l-OTS的含量及光学纯度

谢一凡1，杨若林1，刘慧中2，陆阳1   

  1. 上海交通大学 基础医学院 1.化学教研室， 2.实验教学中心， 上海 200025
  • 出版日期:2016-03-28 发布日期:2017-06-02
  • 通讯作者: 陆阳, 电子信箱: luyangssmu@163.com。
  • 作者简介:谢一凡（1967—）， 男， 高级实验师， 学士; 电子信箱: jyxieyf@shsmu.edu.cn。
  • 基金资助:

    高校教师专业发展计划（BJ13100150032）；国家自然科学基金（81171245）

Determination of l-OTS level and optical purity by ultra performance convergence chromatography method

XIE Yi-fan1, YANG Ruo-lin1, LIU Hui-zhong2, LU Yang1   

  1.  1.Department of Chemistry, 2.ExperimentTeaching Center, Basic Medical Faculty, Shanghai Jiao Tong University, Shanghai 200025, China
  • Online:2016-03-28 Published:2017-06-02
  • Supported by:

    Professional Development Program for University Teachers, BJ13100150032; National Natural Science Foundation of China, 81171245

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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（UPC2）。方法 使用ACQUITY UPC2TM TrefoilTMAMY1手性色谱柱（3.0 mm×50 mm，2.5 μm），柱温30 ℃，以超临界CO2和0.2%二乙胺的异丙醇（95∶5，体积比）为流动相，流速为1.0 mL/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。

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

Abstract:

Objective To develop an ultra performance convergence chromatography (UPC2) 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 TrefoilTMAMY1(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.

Key words: ultra performance convergence chromatography, tropane derivatives, chiral separation, optical purity