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一种同时定量测定延胡索中六种生物碱的 HPLC-MS/MS 方法及其在药代动力学研究中的应用。

A HPLC-MS/MS method for the simultaneous quantitation of six alkaloids of Rhizoma Corydalis Decumbentis in rat plasma and its application to a pharmacokinetic study.

机构信息

College of Science, Nanchang University, No. 999, Xuefu Road, Nanchang 330031, China.

College of Pharmacy, Jilin Medical College, No. 5 Jilin Street, Jilin 132013, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jan 1;944:101-6. doi: 10.1016/j.jchromb.2013.11.010. Epub 2013 Nov 15.

Abstract

A specific and reliable HPLC-MS/MS method was developed and validated for the simultaneous determination of six alkaloids in rat plasma, jatrorrhizine, berberine, tetrahydropalmatine, protopine, bicuculline and palmatine. The analytes were separated on a C18 column (50mm×2.1mm, 1.8μm) and a triple-quadrupole mass spectrometry equipped with an electrospray ionization (ESI) source was used for detection. The plasma sample was prepared by the simple protein precipitation and the recovery for the six analytes was over 80%. The calibration curves were linear over a concentration range of 0.38-1900.0ng/mL for jatrorrhizine, 0.57-2850.0ng/mL for berberine, 0.32-1600.0ng/mL for tetrahydropalmatine, 0.21-1050.0ng/mL for protopine, 0.34-1700.0ng/mL for bicuculline and 0.22-1100ng/mL for palmatine. The intra-day and inter-day precision was less than 15% and the relative error (RE) was all within ±15%. The validated method was successfully applied to a pharmacokinetics study in rats after oral administration of the extracts of Rhizoma Corydalis Decumbentis (a famous Chinese herb).

摘要

建立并验证了一种专属性强、可靠的 HPLC-MS/MS 法,用于同时测定大鼠血浆中的 6 种生物碱,即:延胡索乙素、小檗碱、延胡索甲素、原阿片碱、刻叶紫堇碱和黄连碱。采用 C18 柱(50mm×2.1mm,1.8μm)进行分离,三重四极杆质谱仪,配有电喷雾离子源(ESI)作为检测源。采用简单的蛋白沉淀法处理血浆样品,6 种分析物的回收率均大于 80%。延胡索乙素在 0.38-1900.0ng/mL 浓度范围内、小檗碱在 0.57-2850.0ng/mL 浓度范围内、延胡索甲素在 0.32-1600.0ng/mL 浓度范围内、原阿片碱在 0.21-1050.0ng/mL 浓度范围内、刻叶紫堇碱在 0.34-1700.0ng/mL 浓度范围内、黄连碱在 0.22-1100ng/mL 浓度范围内,均呈现良好的线性关系。日内和日间精密度均小于 15%,相对误差(RE)均在±15%范围内。该方法已成功应用于口服延胡索(一种著名的中药)提取物后的大鼠药代动力学研究。

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