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固相萃取-液相色谱-串联质谱法同时测定乌头侧根中13种氨基醇-二萜生物碱

Simultaneous determination of thirteen aminoalcohol-diterpenoid alkaloids in the lateral roots of Aconitum carmichaeli by solid-phase extraction-liquid chromatography-tandem mass spectrometry.

作者信息

Ding Jia-Yu, Liu Xiu-Xiu, Xiong Dong-Mei, Ye Li-Ming, Chao Ruo-Bing

机构信息

West China School of Pharmacy, Sichuan University, Chengdu, China.

出版信息

Planta Med. 2014 Jun;80(8-9):723-31. doi: 10.1055/s-0034-1368550. Epub 2014 Jun 12.

Abstract

Aminoalcohol-diterpenoid alkaloids have been reported as the cardioactive components in the lateral roots of Aconitum carmichaeli (Fuzi) according to recent studies. Determination of these effective components is of great significance for quality control purposes for Fuzi. Here we report, for the first, the development and validation of a new method to determine the 13 aminoalcohol-diterpenoid alkaloids in Fuzi by using a simple and accurate solid-phase extraction-liquid chromatography-tandem mass spectrometry. The chromatographic analysis was performed on an ODS column with methanol-0.1 % formic acid (80 : 20, v/v) as the mobile phase. The quantification was performed using MS/MS detection in the positive ion mode with multiple reaction monitoring. Linearity was observed within a range of concentrations of 20-2,000 ng/mL. For all the analytes, the r value was greater than 0.9990. The limit of detection and the limit of quantitation were less than 0.5 ng/mL and 2.0 ng/mL, respectively. The intraday and interday precisions were less than 5% and 10%, respectively. The accuracy was within the range of 90 to 105%. This method was successfully applied to determine the 13 aminoalcohol-diterpenoid alkaloids in Fuzi from different origins and with different processing methods.

摘要

根据最近的研究,氨基醇二萜生物碱已被报道为附子(乌头侧根)中的心脏活性成分。测定这些有效成分对于附子的质量控制具有重要意义。在此,我们首次报道了一种通过简单准确的固相萃取-液相色谱-串联质谱法测定附子中13种氨基醇二萜生物碱的新方法的开发与验证。色谱分析在ODS柱上进行,以甲醇-0.1%甲酸(80:20,v/v)作为流动相。定量采用正离子模式下的MS/MS检测和多反应监测。在20-2000 ng/mL的浓度范围内观察到线性关系。对于所有分析物,r值均大于0.9990。检测限和定量限分别小于0.5 ng/mL和2.0 ng/mL。日内和日间精密度分别小于5%和10%。准确度在90%至105%范围内。该方法成功应用于测定不同产地和不同加工方法的附子中13种氨基醇二萜生物碱。

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