UHPLC-MS/MS法在医院制剂多成分含量测定中的应用

doi:10.5246/jcps.2014.04.032

中国药学(英文版) ›› 2014, Vol. 23 ›› Issue (4): 233-240.DOI: 10.5246/jcps.2014.04.032

UHPLC-MS/MS法在医院制剂多成分含量测定中的应用

林志燕, 杨荣富, 唐跃年, 田怀平, 张健^*

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:2014-03-12 修回日期:2014-03-24 出版日期:2014-04-28 发布日期:2014-04-10
通讯作者: *Corresponding author. Tel.: 86-21-25077162; 86-21-25077150; E-mail: zj_xhpharm@126.com; zhiyanlin@163.com
作者简介:*Corresponding author. Tel.: 86-21-25077162; 86-21-25077150; E-mail: zj_xhpharm@126.com; zhiyanlin@163.com
基金资助:
Shanghai Science and Technology Commission Research Fund (Grant No. 11DZ1972500), Shanghai Health Bureau of Traditional Chinese Medicine Research Fund (Grant No. 2012G003A) and Shanghai Municipal Education Commission of Outstanding Young Teachers in Special Fund (Grant No. ZZjdyx13092).

Application of UHPLC-MS/MS method in determining the content of multi-ingredient in hospital preparations

Zhiyan Lin, Rongfu Yang, Yuenian Tang, Huaiping Tian, Jian Zhang^*

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

Received:2014-03-12 Revised:2014-03-24 Online:2014-04-28 Published:2014-04-10
Contact: *Corresponding author. Tel.: 86-21-25077162; 86-21-25077150; E-mail: zj_xhpharm@126.com; zhiyanlin@163.com
About author:*Corresponding author. Tel.: 86-21-25077162; 86-21-25077150; E-mail: zj_xhpharm@126.com; zhiyanlin@163.com
Supported by:
Shanghai Science and Technology Commission Research Fund (Grant No. 11DZ1972500), Shanghai Health Bureau of Traditional Chinese Medicine Research Fund (Grant No. 2012G003A) and Shanghai Municipal Education Commission of Outstanding Young Teachers in Special Fund (Grant No. ZZjdyx13092).

摘要/Abstract

摘要：

射干合剂和甘地胶囊是新华医院的两个院内中药复方制剂, 本文建立了UHPLC-MS/MS方法同时测定这两个制剂中的麻黄碱、咖啡酸、阿魏酸、芦丁、野黄芩苷、射干苷、黄芩苷、黄芩素、黄芪甲苷、次野鸢尾黄素、汉黄芩素等11种中药成分的含量。色谱柱采用ZORBAX SB-C₁₈ (2.1 mm × 50 mm, 1.8 μm), 流动相为0.1%甲酸水溶液-乙腈,梯度洗脱, 流速为0.3 mL/min, 柱温35 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, 其中咖啡酸、阿魏酸、野黄芩苷、射干苷采用负离子模式检测, 麻黄碱、芦丁、黄芩苷、黄芩素、黄芪甲苷、次野鸢尾黄素、汉黄芩素采用正离子模式检测。结果显示麻黄碱、咖啡酸、阿魏酸、芦丁、野黄芩苷、射干苷、黄芩苷、黄芩素、黄芪甲苷、次野鸢尾黄素、汉黄芩素的定量限分别为4.90×10^-3 ng/mL、7.80 ng/mL、6.8 ng/mL、5.3×10^-2 ng/mL、4.20×10^-3 ng/mL、4.6×10^-2 ng/mL、1.44×10^-4 ng/mL、4.85 ng/mL、0.23 ng/mL、3.18×10^-4 ng/mL、2.95×10^-4 ng/mL, 检测限分别为2.90×10^-4 ng/mL、0.77 ng/mL、2.0 ng/mL、0.016 ng/mL、1.3×10^-3 ng/mL、3.33×10^-4 ng/mL、4.32×10^-5ng/mL、1.46 ng/mL、0.07 ng/mL、9.5×10^-5 ng/mL、8.84×10^-5 ng/mL。在相应的线性范围内R²>0.99; 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20 min内实现这11种目标化合物的分离和测定, 简单、快速、灵敏、准确,可用于射干合剂和甘地胶囊的指标成分含量测定, 为这两个制剂的质量控制提供依据。

关键词: 射干合剂, 甘地胶囊, 超高压液相色谱-质谱联用, 多成分含量测定, 中药质量控制

Abstract:

In the present study, we established an ultra-high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to simultaneously determine 11 compounds in two hospital preparations(Shegan mixture and Gandi capsules), including ephedrine, caffeic acid, ferulic acid, rutin, scutellarin, belamcandin, baicalin, baicalein, astragaloside IV, irisflorentin and wogonin. The chromatographic separation was conducted on ZORBAX SB-C₁₈ (2.1 mm×50 mm, 1.8 μm). Eleven analytes and IS were detected using ESI and MRM combined with positive and negative scanning switch. Caffeic acid, ferulic acid, scutellarin and belamcandin were detected using negative ion mode detection, whereas ephedrine, rutin, baicalin, baicalein, astragaloside IV, irisflorentin and wogonin were detected using positive ion mode detection. The quantification limits of ephedrine, caffeic acid, scutellarin, belamcandin, baicalin, baicalein, irisflorentin and wogonin were 4.90×10^-3 ng/mL, 7.80 ng/mL, 6.8 ng/mL, 5.3×10^-2 ng/mL, 4.20×10^-3 ng/mL, 4.6×10^-2 ng/mL, 1.44×10^-4 ng/mL, 4.85 ng/mL, 0.23 ng/mL, 3.18×10^-4 ng/mL and 2.95×10^-4 ng/mL, respectively. The detection limits of these components were 2.90×10^-4 ng/mL, 0.77 ng/mL, 2.0 ng/mL, 0.016 ng/mL, 1.3×10^-3 ng/mL, 3.33×10^-4 ng/mL, 4.32×10^-5 ng/mL, 1.46 ng/mL, 0.07 ng/mL, 9.5×10^-5 ng/mL and 8.84×10^-5 ng/mL, respectively. All calibration curves showed good linearity (R²>0.99) within the test range. The RSD values of intra-day and inter-day precision were less than 5%, and the average recovery rates of the 11 components ranged from 80% to 120%. In conclusion, our newly developed method was simple, rapid, sensitive and accurate. It could be used to determineephedrine, caffeic acid, ferulic acid, rutin, scutellarin, belamcandin, baicalin, baicalein, astragaloside IV, irisflorentin and wogonin in Shegan mixture and Gandi capsules, which was helpful for the quality control of drugs.

Key words: Shegan mixture, Gandi capsules, Ultra-high pressure liquid chromatography-tandem mass spectrometry, Determination of multi-ingredient, Quality control of Chinese patent drug

中图分类号:

R917

Supporting: Shanghai Science and Technology Commission Research Fund (Grant No. 11DZ1972500), Shanghai Health Bureau of Traditional Chinese Medicine Research Fund (Grant No. 2012G003A) and Shanghai Municipal Education Commission of Outstanding Young Teachers in Special Fund (Grant No. ZZjdyx13092).

林志燕, 杨荣富, 唐跃年, 田怀平, 张健. UHPLC-MS/MS法在医院制剂多成分含量测定中的应用[J]. 中国药学(英文版), 2014, 23(4): 233-240.

Zhiyan Lin, Rongfu Yang, Yuenian Tang, Huaiping Tian, Jian Zhang. Application of UHPLC-MS/MS method in determining the content of multi-ingredient in hospital preparations[J]. Journal of Chinese Pharmaceutical Sciences, 2014, 23(4): 233-240.

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UHPLC-MS/MS法在医院制剂多成分含量测定中的应用

Application of UHPLC-MS/MS method in determining the content of multi-ingredient in hospital preparations

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