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采用亲水作用色谱-串联三重四极杆质谱法快速定量分析苦参中喹诺里西啶生物碱及其生物合成前体赖氨酸

A simple and fast quantitative analysis of quinolizidine alkaloids and their biosynthetic precursor, lysine, in Sophora alopecuroides by hydrophilic interaction chromatography coupled with triple-quadrupole tandem mass spectroscopy.

机构信息

College of Pharmacy, Ningxia Medical University, Yinchuan, Ningxia, P. R. China.

Ningxia Research Centre of Modern Hui Medicine Engineering and Technology, Ningxia Medical University, Yinchuan, P. R. China.

出版信息

Phytochem Anal. 2018 Sep;29(5):500-506. doi: 10.1002/pca.2757. Epub 2018 Mar 24.

Abstract

INTRODUCTION

Different parts of Sophora alopecuroides L. (Fabaceae) have historically been used in traditional Chinese medicine for the treatment of dysentery and enteritis. This plant is also utilised as an important resource for industrial preparation of quinolizidine alkaloidal pharmaceuticals.

OBJECTIVE

Establish a reliable, simple and fast analytical method for the quantitative determination of the quinolizidine-type alkaloids and extend understanding of the metabolism of quinolizidine-type alkaloids in S. alopecuroides.

METHODS

Hydrophilic interaction chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-TQ-MS/MS) in multiple-reaction monitoring (MRM) mode were used to determine seven quinolizidine-type alkaloids and their biosynthetic precursor, lysine, in S. alopecuroides.

RESULTS

A good separation was obtained on an ultra high-performance liquid chromatography (UHPLC) amide column within 7 min. The overall limits of detection (LODs) were between 1.13 and 2.81 ng/ml, and limits of quantitation (LOQs) were between 3.80 and 8.48 ng/ml. The developed method was successfully applied to 21 samples of S. alopecuroides. The seeds had the highest concentration of alkaloids among the different plant parts. Oxymatrine and oxysophocarpine were the two most abundant alkaloids in all of the different parts and at different phenological growth stages. The contents of quinolizidine alkaloids showed correlations with lysine.

CONCLUSION

A rapid and sensitive analytical method was established for the simultaneous determination of seven quinolizidine-type alkaloids and their biosynthetic precursor, lysine, in S. alopecuroides; the content of lysine may be used as a marker to predict alkaloid production.

摘要

简介

苦参(豆科)的不同部位在传统中药中历来被用于治疗痢疾和肠炎。这种植物也被用作工业制备喹诺里西啶生物碱药物的重要资源。

目的

建立一种可靠、简单、快速的分析方法,定量测定喹诺里西啶型生物碱,并加深对苦参中喹诺里西啶型生物碱代谢的理解。

方法

采用亲水作用色谱-三重四极杆串联质谱(HILIC-TQ-MS/MS)在多重反应监测(MRM)模式下,测定苦参中的 7 种喹诺里西啶型生物碱及其生物合成前体赖氨酸。

结果

在超高效液相色谱(UHPLC)酰胺柱上 7 分钟内获得了良好的分离。总检测限(LOD)在 1.13 至 2.81ng/ml 之间,定量限(LOQ)在 3.80 至 8.48ng/ml 之间。该方法成功应用于 21 个苦参样品。不同植物部位中,种子中的生物碱含量最高。氧化苦参碱和氧化槐果碱是所有不同部位和不同物候生长阶段中含量最丰富的两种生物碱。生物碱含量与赖氨酸呈正相关。

结论

建立了一种快速灵敏的分析方法,可同时测定苦参中的 7 种喹诺里西啶型生物碱及其生物合成前体赖氨酸;赖氨酸的含量可用作预测生物碱产量的标志物。

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