标准研讨

UPLC-MS/MS法测定半枝莲中4个二萜烟酸酯的含量*

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  • 沈阳药科大学药学院,沈阳 110016
第一作者 Tel:13478302684;E-mail:iamyangdoctor@126.com
** Tel:(024)43528600;E-mail:slx04@163.com

收稿日期: 2020-01-13

  网络出版日期: 2024-05-31

基金资助

* 辽宁省教育厅重点项目(2017LZD04); 辽宁特聘教授滚动资助项目(辽教函发[2018]35 号)

Simultaneous determination of four diterpenoid nicotinates in Scutellariae Barbatae Herba by UPLC-MS/MS*

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  • School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China

Received date: 2020-01-13

  Online published: 2024-05-31

摘要

目的:建立同时测定半枝莲中半枝莲碱A、半枝莲碱B、半枝莲萜C 和半枝莲萜F 含量的UPLC-MS/MS 分析方法。方法:采用ACQUITY UPLC® BEH C18 色谱柱(100 mm×2.1 mm,1.7 μm),以0.1% 甲酸水溶液(A)-0.1% 甲酸乙腈(B)为流动相,梯度洗脱(0~7 min,48%B → 100%B;7~8 min,100%B;8~8.5 min,100%B → 48%B;8.5~10 min,48%B),流速0.2 mL·min-1,柱温30 ℃ ;质谱采用电喷雾离子源(ESI),多反应监测(MRM)正离子模式进行扫描。结果:半枝莲碱A、半枝莲碱B、半枝莲萜C、半枝莲萜F 质量浓度分别在0.334 4~13.38、0.223 1~8.923、0.162 4~6.496、0.198 8~7.954 μg·mL-1 的范围内线性关系良好(r 皆大于0.999);平均回收率(n=9)分别为98.2%、98.6%、99.9%、93.3%,RSD 分别为4.2%、6.2%、4.6%、6.3%;27 批样品中上述4 个成分含量范围分别为15.44~168.4、14.98~118.23、13.31~62.40、12.37~117.67 μg·g-1结论:所建立的方法可用于半枝莲中主要二萜烟酸酯类成分的定量分析。

本文引用格式

杨国春, 吕星, 林紫薇, 孙立新 . UPLC-MS/MS法测定半枝莲中4个二萜烟酸酯的含量*[J]. 药物分析杂志, 2021 , 41(1) : 130 -137 . DOI: 10.16155/j.0254-1793.2021.01.16

Abstract

Objective: To establish a quantitative method for the determination of scutebarbatine A,scutebarbatine B,scutebata C and scutebata F in Scutellariae Barbatae Herba by UPLC-MS/MS. Methods: The determination was performed on an ACQUITY UPLC® BEH C18(2.1 mm×100 mm,1.7 μm)at 30 ℃ . The mobile phase of 0.1% formic acid solution(A)-0.1% formic acid acetonitrile(B)was subjected to gradient elution(0-7 min, 48%B → 100%B;7-8 min,100%B;8-8.5 min,100%B → 48%B;8.5-10 min,48%B)at the flow rate of 0.2 mL· min-1. The analytes were determined by electrospray ionization source(ESI)combined with multiple reaction monitoring (MRM)in positive ion mode. Results: Scutebarbatine A showed a good linearity in the range of 0.334 4- 13.38 μg· mL-1(r>0.999),scutebarbatine B showed a good linearity in the range of 0.223 1-8.923 μg·mL-1(r>0.999), scutebata C showed a good linearity in the range of 0.162 4-6.496 μg·mL-1(r>0.999),and scutebata F showed a good linearity in the range of 0.198 8-7.954 μg·mL-1(r>0.999). The average recoveries(n=9)were 98.2%, 98.6%,99.9% and 93.3%,and the corresponding RSDs were 4.2%,6.2%,4.6% and 6.3%,respectively. The contents of scutebarbatine A,scutebarbatine B,scutebata C and scutebata F in 27 batches of samples were 15.44- 168.4,14.98-118.23,13.31-62.40,12.37-117.67 μg·g-1,respectively. Conclusion: The method is competent in the quantification of the main diterpenoid nicotinates in Scutellariae Barbatae Herba.

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