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以手性离子液体和羟丙基-β-环糊精为添加剂,采用毛细管电泳中的场放大进样堆积法分离测定钩藤碱和异钩藤碱。

Separation and determination of corynoxine and corynoxine B using chiral ionic liquid and hydroxypropyl-β-cyclodextrin as additives by field-amplified sample stacking in capillary electrophoresis.

作者信息

Wang Zhiying, Guo Haitao, Chen Meng, Zhang Guangbin, Chang Ruimiao, Chen Anjia

机构信息

College of Pharmacy, Shanxi Medical University, Taiyuan, P. R. China.

出版信息

Electrophoresis. 2018 Sep;39(17):2195-2201. doi: 10.1002/elps.201800129. Epub 2018 Jul 8.

Abstract

A sensitive, fast, and effective method, field-amplified sample stacking (FASS) in capillary electrophoresis, has been established for the separation and determination of corynoxine and corynoxine B. Hydroxypropyl-β-CD (HP-β-CD) and tetrabutylammonium-L-glutamic acid (TBA-L-Glu) were used as additives in the separation system. Electrokinetic injection was chosen to introduce sample from inlet at 10 kV for 50 s after a water plug (0.5 psi, 4 s) was injected to permit FASS. The running buffer (pH 6.1) was composed of 40 mM sodium dihydrogen phosphate solution, 130 mM HP-β-CD, and 10 mM TBA-L-Glu and the separation voltage was 20 kV. Under the optimum conditions, corynoxine and corynoxine B were successfully enriched and separated within 12 min and the sensitivity was improved approximately by 700-900 folds. Calibration curves were in a good linear relationship within the range of 62.5-5.00 × 10  ng/mL for both corynoxine and corynoxine B. The limits of detection (S/N = 3) and quantitation (S/N = 10) were 14.9, 45.2 ng/mL for corynoxine and 11.2, 34.5 ng/mL for corynoxine B, respectively. Finally, this method was successfully applied for the determination of corynoxine and corynoxine B in the stems with hooks of Uncaria rhynchophylla and its formulations.

摘要

已建立一种灵敏、快速且有效的方法——毛细管电泳中的场放大进样堆积(FASS),用于分离和测定钩藤碱和异钩藤碱。羟丙基-β-环糊精(HP-β-CD)和四丁基铵-L-谷氨酸(TBA-L-Glu)用作分离体系中的添加剂。选择电动进样,在注入水塞(0.5 psi,4 s)以实现FASS后,于10 kV下从进样口引入样品50 s。运行缓冲液(pH 6.1)由40 mM磷酸二氢钠溶液、130 mM HP-β-CD和10 mM TBA-L-Glu组成,分离电压为20 kV。在最佳条件下,钩藤碱和异钩藤碱在12分钟内成功富集并分离,灵敏度提高了约700 - 900倍。钩藤碱和异钩藤碱在62.5 - 5.00×10 ng/mL范围内校准曲线呈良好线性关系。钩藤碱的检测限(S/N = 3)和定量限(S/N = 10)分别为14.9、45.2 ng/mL,异钩藤碱的检测限和定量限分别为11.2、34.5 ng/mL。最后,该方法成功应用于钩藤及其制剂带钩茎中钩藤碱和异钩藤碱的测定。

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