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采用超高效液相色谱-电喷雾串联质谱和飞行时间质谱法对中华酸模叶蓼(中国灯笼)中主要活性物 physalins 的定量和转化产物分析。

Quantitative and transformation product analysis of major active physalins from Physalis alkekengi var. franchetii (Chinese lantern) using ultraperformance liquid chromatography with electrospray ionisation tandem mass spectrometry and time-of-flight mass spectrometry.

机构信息

College of Pharmaceutical Sciences, Zhejiang University, 338 Yuhangtang Road, Hangzhou 310058, China.

出版信息

Phytochem Anal. 2012 Jul-Aug;23(4):337-44. doi: 10.1002/pca.1363. Epub 2011 Oct 13.

Abstract

INTRODUCTION

Chinese lantern is the calyx or calyx-with-fruit of the plant Physalis alkekengi .var. franchetii (Solanaceae), and is potential material for the food and pharmaceutical industries. Physalins are the most active and representative secondary metabolites of Chinese lantern. A separation and quantification method based on UPLC-ESI-MS/MS was developed for the quantitative analysis of five active physalins. The transformation products were also detected and identified for the first time.

OBJECTIVE

To establish a LC-MS/MS method to quantify five physalins in Chinese lantern for the purpose of quality control, and to identify the transformation products of 4,7-didehydrophysalin B.

METHODOLOGY

The separation was carried out on an Acquity UPLC BEH Shield RP C₁₈-column with water and acetonitrile as the mobile phase under gradient conditions. ESI-MS/MS was used as the detector to quantify the five physalins. The transformation products of 4,7-didehydroneophysalin B were detected by UPLC-PDA-ESI-MS/MS and identified through comparing their HRMS and MS² ion fragmentations with corresponding references.

RESULTS

All the compounds showed good linearity (R²  > 0.998). The recoveries, measured at three concentration levels, varied from 98.8 to 101.4% with RSDs < 4.5%. The total contents of the five physalins in Chinese lantern varied significantly. Three transformation products of 4,7-didehydroneophysalin B were detected and tentatively identified.

CONCLUSION

The present study developed a highly effective analytical method for the quality control of Chinese lantern, and it could provide comprehensive information for quality evaluation and new drug development of Chinese lantern.

摘要

简介

灯笼草是茄科酸浆属植物酸浆Physalis alkekengi.var. franchetii 的宿萼或带果宿萼,是食品和医药工业的潜在原料。茄烷类是灯笼草中最活跃和最具代表性的次生代谢物。建立了基于 UPLC-ESI-MS/MS 的分离和定量分析方法,用于五种活性茄烷的定量分析。首次检测并鉴定了转化产物。

目的

建立 LC-MS/MS 法测定灯笼草中五种茄烷的含量,为质量控制提供依据,并鉴定 4,7-二脱氢灯笼草 B 的转化产物。

方法

采用 Acquity UPLC BEH Shield RP C₁₈ 柱,以水和乙腈为流动相,梯度洗脱,ESI-MS/MS 作为检测器进行定量分析。采用 UPLC-PDA-ESI-MS/MS 检测 4,7-二脱氢灯笼草 B 的转化产物,并通过比较其高分辨质谱和 MS² 离子碎片与相应参考文献来鉴定。

结果

所有化合物均呈良好的线性关系(R²  > 0.998)。在三个浓度水平下测定的回收率在 98.8%至 101.4%之间,RSDs<4.5%。灯笼草中五种茄烷的总含量差异较大。检测到并初步鉴定了 4,7-二脱氢灯笼草 B 的三种转化产物。

结论

本研究建立了一种高效的分析方法,用于灯笼草的质量控制,可为灯笼草的质量评价和新药开发提供全面信息。

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