高效液相色谱-电雾式检测器测定牛黄解毒片中的6种胆汁酸

林楚慧 柴瑞平 张璐 付志博 章弘扬 张敏 胡坪

引用本文: 林楚慧, 柴瑞平, 张璐, 付志博, 章弘扬, 张敏, 胡坪. 高效液相色谱-电雾式检测器测定牛黄解毒片中的6种胆汁酸[J]. 分析化学, 2022, 50(5): 764-771. doi: 10.19756/j.issn.0253-3820.210910 shu
Citation:  LIN Chu-Hui,  CHAI Rui-Ping,  ZHANG Lu,  FU Zhi-Bo,  ZHANG Hong-Yang,  ZHANG Min,  HU Ping. Determination of Six Kinds of Bile Acids in NiuhuangJiedu Tablets Using High Performance Liquid Chromatography Coupled with Charged Aerosol Detector[J]. Chinese Journal of Analytical Chemistry, 2022, 50(5): 764-771. doi: 10.19756/j.issn.0253-3820.210910 shu

高效液相色谱-电雾式检测器测定牛黄解毒片中的6种胆汁酸

    通讯作者: 胡坪,E-mail:huping@ecust.edu.cn
  • 基金项目:

    国家自然科学基金项目(No.81973285)资助。

摘要: 建立了牛黄解毒片中6种胆汁酸类物质(甘氨胆酸、猪脱氧胆酸、胆酸、甘氨脱氧胆酸、鹅脱氧胆酸与脱氧胆酸)的高效液相色谱-电雾式检测器(HPLC-CAD)测定方法。样品经70%(V/V)甲醇超声提取,氮吹浓缩后,以Agilent Poroshell 120 EC C18色谱柱(100 mm × 4.6 mm,2.7 μm)分离,采用甲醇和5 mmol/L乙酸铵-0.1%甲酸溶液梯度洗脱,设置电雾式检测器的雾化温度为55℃,幂律参数(PFV)为1.35。甘氨胆酸、猪脱氧胆酸、胆酸、甘氨脱氧胆酸、鹅脱氧胆酸和脱氧胆酸分别在2.10~972 μg/mL、2.09~1046 μg/mL、2.05~978 μg/mL、2.56~1022 μg/mL、1.25~658 μg/mL和2.05~1025 μg/mL浓度范围内线性良好,相关系数(R2)大于0.9991,检出限在0.86~1.53 μg/mL之间,定量限在1.20~2.56 μg/mL之间,平均回收率在94.2%~105.3%之间,相对标准偏差(RSD)小于1.6%。将本方法应用于实际牛黄解毒片样品的测定,结果表明,不同厂家生产的牛黄解毒片中胆汁酸的含量差异显著。建立的6种胆汁酸的HPLC-CAD含量测定方法灵敏、准确、可靠,可用于中药复方牛黄解毒片质量评价。

English


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  • 收稿日期:  2021-12-31
  • 修回日期:  2022-02-27
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