首页|UPLC-Q-Exactive-Orbitrap-MS法同时测定牛黄上清片中18种胆汁酸的含量

UPLC-Q-Exactive-Orbitrap-MS法同时测定牛黄上清片中18种胆汁酸的含量

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目的 建立超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Exactive-Orbitrap-MS)法同时测定牛黄上清片中牛磺胆酸、7-酮-3α,12-α-羟基胆烷酸、甘氨猪去氧胆酸、12-脱氢胆酸、甘氨胆酸、3-酮-7α,12α-二羟基-5β-胆烷酸、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、石胆酸的含量.方法 分析采用 Thermo Fisher Scientfic Bremen HYPERSIL GOLD色谱柱(2.1 mm×100 mm,1.9 μm);流动相0.1%甲酸-甲醇,梯度洗脱;体积流量0.2 mL/min;柱温 40℃;加热电喷雾离子源;负离子扫描;平行反应监测模式.再进行化学模式识别.结果 18 种胆汁酸在各自范围内线性关系良好(r≥0.999 5),平均加样回收率 96.73%~104.07%,RSD 2.10%~4.07%.不同厂家样品中各胆汁酸在种类和含量上存在一定差异.结论 该方法灵敏可靠,专属性好,可用于牛黄上清片的质量控制.
Simultaneously content determination of eighteen bile acids in Niuhuang Shangqing Tablets by UPLC-Q-Exactive-Orbitrap-MS
AIM To establish a ultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry(UPLC-Q-Exactive-Orbitrap-MS)method for the simultaneous content determination of taurocholic acid,7-ketodeoxycholic acid,glycohyodeoxycholic acid,12-oxochenodeoxycholic acid,gycocholic acid,3-oxo-7α,12α-hydroxy-5β-cholanoic acid,taurochenodeoxycholic acid,3-oxocholic acid,hyocholic acid,taurodeoxycholic acid sodium salt hydrate,hyodeoxycholic acid,cholic acid,gycochenodeoxycholic acid,glycodesoxycholic acid,taurolithocholic acid sodium salt,ghenodeoxycholic acid,deoxycholic acid and lthocolic acid in Niuhuang Shangqing Tablets.Then chemical pattern recognition was performed.METHODS The analysis was performed on a 40℃thermostatic Thermo Fisher Scientfic Bremen HYPERSIL GOLD column(2.1 mm×100 mm,1.9 μm),with the mobile phase comprising of 0.1%formic acid-methanol flowing at 0.2 mL/min in a gradient elution manner,and heating electron spray ionization source was adopted in negative ion scanning with parallel reaction monitoring mode.RESULTS Eighteen bile acids showed good linear relationships within their own ranges(r≥0.999 5),whose average recoveries were 96.73%-104.07%with the RSDs of 2.10%-4.07%.Certain differences in kind and content of bile acids in samples from different manufacturers were observable.CONCLUSION This sensitive,reliable and specific method can be used for the quality control of Niuhuang Shangqing Tablets.

Niuhuang Shangqing Tabletsbile acidscontent determinationultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry(UPLC-Q-Exactive-Orbitrap-MS)chemical pattern recognition

林晨、洪芳、陈俊裕、林诗铃、郑燕芳、黄鸣清

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福建省食品药品质量检验研究院, 福建 福州 350012

福建中医药大学, 福建 福州 350122

牛黄上清片 胆汁酸 含量测定 超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Exactive-Orbitrap-MS) 化学模式识别

国家自然科学基金面上项目国家自然科学基金面上项目福厦泉国家自主创新示范区协同创新平台专项

81973437822740802021FX02

2024

中成药
国家食品药品监督管理局,信息中心中成药信息站,上海中药行业协会

中成药

CSTPCD北大核心
影响因子:1.217
ISSN:1001-1528
年,卷(期):2024.46(4)
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