UHPLC-MS/MS法同时测定舒肝祛脂胶囊中4种皂苷的含量

doi:10.5246/jcps.2015.05.041

中国药学(英文版) ›› 2015, Vol. 24 ›› Issue (5): 318-325.DOI: 10.5246/jcps.2015.05.041

UHPLC-MS/MS法同时测定舒肝祛脂胶囊中4种皂苷的含量

林志燕¹, 杨荣富², 唐跃年¹, 田怀平¹, 刘昕竹¹, 陆晓彤^1*

1. 上海交通大学医学院附属新华医院, 上海 200092
2. 上海计划生育科学研究所, 上海 200032

收稿日期:2014-12-29 修回日期:2015-01-25 出版日期:2015-05-20 发布日期:2015-02-10
通讯作者: Tel.: 86-21-25077156, 86-21-25077152
基金资助:
Shanghai Municipal Commission of Health and Family Planning Chinese Medicine Research and Development Fund (Grant No. 2014XP001A); Shanghai Health Bureau of Traditional Chinese Medicine Research Fund (Grant No. 2012G003A); Shanghai Municipal Education Commission of outstanding young teachers in special fund(Grant No. ZZjdyx13092).

Simultaneous determination of four saponins in Shugan Quzhi Capsule by UHPLC-MS/MS

Zhiyan Lin¹, Rongfu Yang², Yuenian Tang¹, Huaiping Tian¹, Xinzhu Liu¹, Xiaotong Lu^1*

1. Department of Pharmacy, Xinhua Hospital Affiliated to School of Medicine, Shanghai Jiaotong University, Shanghai 200092
2. Shanghai Institute of Planned Parenthood Research, Shanghai 200032

Received:2014-12-29 Revised:2015-01-25 Online:2015-05-20 Published:2015-02-10
Contact: Tel.: 86-21-25077156, 86-21-25077152
Supported by:
Shanghai Municipal Commission of Health and Family Planning Chinese Medicine Research and Development Fund (Grant No. 2014XP001A); Shanghai Health Bureau of Traditional Chinese Medicine Research Fund (Grant No. 2012G003A); Shanghai Municipal Education Commission of outstanding young teachers in special fund(Grant No. ZZjdyx13092).

摘要/Abstract

摘要：

舒肝祛脂胶囊是新华医院的院内中药复方制剂, 临床主要用于脂肪肝引起的转氨酶升高和肝内脂肪浸润, 肥胖、高血脂等疾病治疗。本文建立了一种UHPLC-MS/MS方法可同时测定舒肝祛脂胶囊中的三七皂苷R1、人参皂苷Rb1、人参皂苷Re、人参皂苷Rg1等4种三七皂苷成分的含量。色谱柱采用ZORBAX SB-C₁₈(2.1 mm×50 mm, 1.8 μm), 流动相为(0.05%甲酸 + 5 mM醋酸铵)水溶液–乙腈, 梯度洗脱, 流速为0.3 mL/min, 柱温40 ºC; 质谱采用电喷雾离子源(ESI), 多反应离子监测(MRM), 并结合正负离子扫描切换, 其中人参皂苷Re、人参皂苷Rg1采用负离子模式检测, 三七皂苷R1、人参皂苷Rb1及内标人参皂苷F1采用正离子模式检测。结果显示三七皂苷R1、人参皂苷Rb1、人参皂苷Re、人参皂苷Rg1的定量限分别为6.54×10^–4 ng/mL、2.57×10^–4 ng/mL、0.11 ng/mL、6.91×10^–3 ng/mL, 检测限分别为1.96×10^–4 ng/mL、7.70×10^–5ng/mL、3.45×10^–2ng/mL、2.07×10^–3 ng/mL。在相应的线性范围内r²>0.9633; 日内和日间精密度(RSD)均小于5%, 平均回收率均在80%–120%。本方法在6 min内实现这4种皂苷成分的分离和测定, 简单、快速、灵敏、准确, 可用于舒肝祛脂胶囊中皂苷类成分的含量测定。

关键词: 舒肝祛脂胶囊, 超高压液相色谱-质谱联用, 皂苷, 含量测定

Abstract:

Shugan Quzhi capsule is a hospital preparation of Xinhua Hospital affiliated to School of Medicine, Shanghai Jiaotong University. It has been used for the treatment of adult patients with fatty liver caused by obesity, high cholesterol and other factors. In the present study, we established an ultra-high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to simultaneously determine 4 saponiningredients including Notoginsenoside R1, Ginsenoside Rb1, Ginsenoside Re and Ginsenoside Rg1 present in Shugan Quzhi capsule. The chromatographic separation was conducted on ZORBAX SB-C₁₈ (2.1 mm×50 mm, 1.8 μm). The mobile phase was composed of acetonitrile and aqueous solution consisted of 0.05% formic acid and 5 mM ammonium acetate. Gradient elution rate was 0.3 mL/min, the column temperature was 40 ºC; MS was conducted using electrospray ionisation (ESI) and multiple reaction monitoring (MRM) coupled with positive and negative scanning switch. With which, Ginsenoside Re and Ginsenoside Rg1 were detected using negative ion mode detection while Notoginsenoside R1, Ginsenoside Rb1 and internal standard (Ginsenoside F1) were detected using positive ion mode detection. The limits of quantification (LOQ) for Notoginsenoside R1, Ginsenoside Rb1, Ginsenoside Re and Ginsenoside Rg1 were 6.54×10^–4, 2.57×10^–4, 0.11 and 6.91×10^–3 ng/mL, respectively. The limits of detection (LOD) for these compounds were 1.96×10^–4, 7.70×10^–5, 3.45×10^–2, and 2.07×10^–3 ng/mL, respectively. All calibration curves showed a good linearity (r²>0.9633) within the test range. The intra- and inter-day precisions (relative standard deviation, RSD) were lower than 5% and the average recoveries were in the range of 80%–120%. With this method, four kinds of saponins were separated and detected in 6 min. This method is simple, rapid and shows high sensitivity and accuracy.

Key words: Shugan Quzhi capsule, Ultra-high pressure liquid chromatography-tandem mass spectrometry, Saponins, Content determination

中图分类号:

R917

Supporting:

林志燕, 杨荣富, 唐跃年, 田怀平, 刘昕竹, 陆晓彤. UHPLC-MS/MS法同时测定舒肝祛脂胶囊中4种皂苷的含量[J]. 中国药学(英文版), 2015, 24(5): 318-325.

Zhiyan Lin, Rongfu Yang, Yuenian Tang, Huaiping Tian, Xinzhu Liu, Xiaotong Lu. Simultaneous determination of four saponins in Shugan Quzhi Capsule by UHPLC-MS/MS[J]. Journal of Chinese Pharmaceutical Sciences, 2015, 24(5): 318-325.

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UHPLC-MS/MS法同时测定舒肝祛脂胶囊中4种皂苷的含量

Simultaneous determination of four saponins in Shugan Quzhi Capsule by UHPLC-MS/MS

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