非水毛细管电泳内标法测定麻黄中麻黄碱的含量(1)
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[摘要] 目的：以品红为内标，建立非水毛细管电泳(NACE)内标法测定麻黄中麻黄碱的含量。方法：采用毛细管区带电泳分离模式，以30 mmol/L的醋酸铵和醋酸钠甲醇溶液为运行缓冲液，品红为内标物，操作电压20 kV，电迁移进样10 kV×10 s，检测波长为210 nm。结果：麻黄碱在3.125～200.000 mg/L(相关系数r=0.994 0)范围内有良好的线性关系，最低检测限为2.0 mg/L，仪器精密度为2.05%，方法精密度为3.17%，回收率为97.47%～101.85%。结论：此方法为麻黄碱的测定提供了一种简便、快速、定量可靠的方法，可用于医学研究样品和药材中麻黄碱的测定。
[关键词] 非水毛细管电泳；内标；品红；麻黄碱
[中图分类号] R917 [文献标识码] A [文章编号] 1673-7210(2011)12(b)-072-03
Determination of ephedrine in ephedras by nonaqueous capillary electrophoresis by internal standard method
XIAO Yuhang1, QIN Qun1, JING Zhaozheng2
1.Department of Pharmacy, Xiangya Hospital, Central South University, Hu′nan Province, Changsha 410008, China; 2.Department of the Central Laboratory, Xiangya Hospital, Central South University, Hu′nan Province, Changsha 410008, China
[Abstract] Objective: To establish nonaqueous capillary electrophoresis (NACE) method for the determination of ephedrine in ephedras by internal standard with fuchsin was the internal standard sample. Methods: Based on the mode of capillary zone electrophoresis (CZE) electrophoretic separation, 30 mmol/L ammonium acetate and sodium acetate as the running buffer and fuchsin as the internal standard sample were used, with a constant voltage was 20 kV, electromigration injection was 10 kV×10 s and detection wavelength was 210 nm. Results: Linearity was obtained in the range of 3.125-200.000 mg/L for ephedrine (r=0.994 0). The LLOQ was 2.0 mg/L, instrument precision was 2.05%, method precision was 3.17%, and the recovery rate was 97.47%-101.85%. Conclusion: This method, with an adequate internal standard and non-aqueous electrophoresis medium, optimized equipment parameters and simplified pretreatment procedure, is convenient, rapid, quantitative and reliable for determining ephedrine, and also can be used for the determination of ephedrine in medical samples and herbs.
[Key words] Nonaqueous capillary electrophoresis; Internal standard; Fuchsin; Ephedrine
麻黄碱(ephedrine)是中药麻黄的主要有效成分，具有松弛支气管平滑肌、扩张支气管、收缩血管、升高血压及兴奋中枢等作用。麻黄碱的测定方法很多，除容量分析法外，还包括薄层扫描法[1]、高效液相色谱法[2-4]、气相色谱法[5]、电位滴定法以及导数光谱[6]、双波长[7]等各种紫外分光光度法。目前高效毛细管电泳法已广泛应用于中药成分的分析[8]，相比以上所述分析方法，它具有分析周期短，柱子不易污染，消耗试剂少，费用低的优点，特别适用于快速检验。目前也有毛细管电泳方法用于测定麻黄碱的报道[9-10]。本文采用非水毛细管电泳内标法定量测定麻黄碱 ......
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