摘要
采用超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法(UPLC-Q Exactive-Orbitrap MS)进行牛黄降压丸中15种成分(牛磺胆酸、7-酮-3α,12-α-羟基胆烷酸、甘氨胆酸、3-氧代脱氧胆酸、牛磺鹅去氧胆酸、3α-羟基-7-氧代-5β-胆烷酸、猪胆酸、牛磺脱氧胆酸钠、猪去氧胆酸、胆酸、甘氨鹅脱氧胆酸、甘氨脱氧胆酸、牛磺石胆酸钠、鹅去氧胆酸、去氧胆酸)的含量测定。色谱条件:采用Thermo Fisher Scientfic Bremen HYPERSIL GOLD(100 mm×2.1 mm,1.9μm)色谱柱,以0.1%甲酸水-甲醇为流动相,进行梯度洗脱;质谱采用加热电喷雾离子源(HESI)负离子模式,平行反应监测(PRM)扫描模式测定数据。结果表明,15种胆酸类成分在各自的质量浓度范围内具有良好的线性关系(r≥0.9990),加样回收率均在93.7%~105.2%之间(n=9)。采用建立好的方法测定15批样品的含量,结果表明不同批次牛黄降压丸中胆酸类成分的含量差异较大。本研究为牛黄降压丸的全面质量控制提供究提供思路及参考。
An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q Exactive-Orbitrap MS)method for the simultaneous determination of 15 compounds(taurocholic acid,7-keto-3α,12-α-dihydroxycholanic acid,glycocholic acid,3-oxo-7α,12α-hydroxy-5β-cholanoic acid,taurochenodeoxycholic acid,3α-hydroxy-7-oxo-5β-cholanic acid,hyocholic acid,sodium taurodeoxycholate,hyodeoxycholic acid,cholic acid,glycochenodeoxycholic acid,glycodeoxycholic acid,taurolithocholic acid sodium salt,chenodeoxycholic acid,deoxycholic acid)in Niuhuang Jiangya Pills was established.The separation was performed on a Thermo Fisher Scientfic Bremen HYPERSIL GOLD C18 column(100 mm×2.1 mm,1.9μm).Methanol and water(containing 0.1%formic acid)were adopted as the mobile phase by gradient elution.MS detection was performed with multiple reaction monitoring mode.The results showed that fifteen compounds had a good linearity within their respective concentration ranges(r>0.9990).The average recovery rates were 93.7%-105.2%(n=9).The established method was used to determine the content of 15 batches of samples,and the results showed that the content of cholic acid was quite different.The present study provides an important reference for the overall quality control of Niuhuang Jiangya Pills.
作者
黄秋妹
林诗铃
石茗
郑燕芳
黄鸣清
HUANG Qiu-mei;LIN Shi-ling;SHI Ming;ZHENG Yan-fang;HUANG Ming-qing(Guangdong Food and Drug Vocational College,Guangzhou 510520,China;School of Pharmacy,Fujian University of Traditional Chinese Medicine,Fuzhou 350122,China)
出处
《药学学报》
CAS
CSCD
北大核心
2023年第9期2777-2784,共8页
Acta Pharmaceutica Sinica
基金
国家自然科学基金面上项目(81973437,82274080)
福厦泉国家自主创新示范区协同创新平台专项(2021FX02)。
