UPLC-MS/MS法测定五倍子洗剂中5种指标性成分的含量 |
投稿时间:2021-02-28 修订日期:2021-05-13 点此下载全文 |
引用本文:张群,陈瑜,支晓伟,须秋萍,杨英楠,赵亮,李盛建.UPLC-MS/MS法测定五倍子洗剂中5种指标性成分的含量[J].药学实践杂志,2021,39(5):437~441 |
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基金项目:宝山区医学特色专科和社区项目建设课题(BSZK-2018-A10, BSZK-2019-C03);宝山区罗店医院科研课题(20-A-6) |
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中文摘要:目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时检测五倍子洗剂中没食子酸、紫丁香苷、黄柏碱、秦皮乙素、大黄酸的含量。方法 采用UPLC-MS/MS法,色谱柱为Agilent Poroshell 120 EC-C18(2.1 mm×150 mm,2.7 μm),流动相为0.2%甲酸溶液-乙腈,梯度洗脱,流速为0.3 ml/min,柱温30 ℃;进样量2 μl。质谱检测采用动态多反应离子检测模式(DMRM)。结果 没食子酸、紫丁香苷、黄柏碱、秦皮乙素、大黄酸分别在153.8~15380、10.31~1031、5.265~526.5、50.70~5070、1.054~105.4 ng/ml浓度范围内线性关系良好,其精密度、重复性、稳定性和加样回收率均良好。结论 该UPLC-MS/MS法稳定、快速、重复性好,适用于检测五倍子洗剂中没食子酸、紫丁香苷、黄柏碱、秦皮乙素、大黄酸的含量。 |
中文关键词:超高效液相色谱-串联质谱法 五倍子洗剂 含量测定 |
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Quantitative analysis of five compounds in gallnut lotion by UPLC-MS/MS |
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Abstract:Objective To develop an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to simultaneously detect the contents of gallic acid, syringin, phellodendrine, aesculin and rhein in the gallnut lotion.Methods An UPLC- MS/MS method was established. Separation was performed on an Agilent Poroshell 120 EC-C18(2.1 mm×150 mm, 2.7 μm)with a gradient mobile phase system of 0.2% formic water-acetonitrile solution. The flow rate was 0.3 ml/min. The temperature of column was 30 ℃. The injection volume was 2 μl. The MS detection was in dynamic MRM mode.Results gallic acid, syringin, phellodendrine, aesculin and rhein were successfully separated using this method, with good linear relationship as the ranges of 153.8-15380、10.31-1031、5.265-526.5、50.70-5070、1.054-105.4 ng/ml, respectively. The precision, repeatability, stability and recovery were good.Conclusion This UPLC-MS/MS method is stable, rapid, and reproducible., It is suitable for detecting the contents of gallic acid, syringin, phellodendrine, esculetin and in the gallnut lotion. |
keywords:UPLC- MS/MS gallnut lotion determination |
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