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UPLC-MS/MS法同时测定排石合剂中10个特征成分含量

Simultaneous determination of 10 representative components in Paishi mixture by UPLC/MS/MS

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【作者】 李均艳李舒琪刘辉王芝燕何一琴刘永利

【Author】 LI Jun-yan;LI Shu-qi;LIU Hui;WANG Zhi-yan;HE Yi-qin;LIU Yong-li;Wujin Traditional Chinese Medicine Hospital of Changzhou City;Hebei University of Chinese Medicine;Hebei Institute for Drug and Medical Device Control;

【通讯作者】 刘辉;刘永利;

【机构】 常州市武进中医医院河北中医药大学河北省药品医疗器械检验研究院

【摘要】 目的:建立UPLC-MS/MS法同时测定排石合剂中京尼平苷酸、羟基红花黄色素A、绿原酸、苦杏仁苷、王不留行黄酮苷、甘草苷、毛蕊花糖苷、杯苋甾酮、丹皮酚、甘草酸铵10个特征成分的含量。方法:供试品经70%甲醇超声处理,Waters HSS T3 C18(100 mm×2.1 mm, 1.7μm)色谱柱,以乙腈-0.1%甲酸为流动相进行梯度洗脱,流速0.3 mL·min-1;电喷雾正负离子源同时监测,多反应监测(MRM)模式。结果:方法重复性、准确度良好,10个成分的平均回收率在99.0%~101.0%,RSD为0.090%~4.3%,在各自浓度范围内线性关系良好,含量结果分别为31.129~34.256、95.456~98.741、126.85~129.43、238.62~240.90、45.620~47.520、26.124~28.412、13.852~15.030、16.632~17.854、800.41~805.56、78.485~80.963μg·mL-1。结论:本研究建立的方法快速简便,选择性好,准确可靠,为排石合剂的质量控制提供科学依据。

【Abstract】 Objective:To establish simultaneous determination method of 10 representative components in Paishi mixture, including geniposidic acid, hydroxyl-safflor yellow A, chlorogenic acid, amygdalin, vaccarin, liquiritin, mulberry glycoside, cyclamenone, paeonol and ammonium glycyrrhizinate. Methods: The sample was ultrasonicated with 70% methanol. The chromatographic separation was performed on a Waters HSS T3 C18(100 mm×2.1 mm, 1.7 μm)column with acetonitrile-0.1% formic acid solution as mobile phase with gradient elution. The flow rate was 0.3 mL·min-1. The analytes were detected by tandem mass spectrometry under the positive and negative ion modes with the ESI source and multiple reaction monitoring(MRM) mode. Results: The repeatability and accuracy of the method were good, and the average recoveries were 99.0%-101.0% with RSDs of0.090%-4.3%. The sample determination results showed that there were differences in the consistency between batches of preparations. The contents of 10 components were 31.129-34.256, 95.456-98.741, 126.85-129.43, 238.62-240.90, 45.620-47.520, 26.124-28.412, 13.852-15.030, 16.632-17.854, 800.41-805.56, 78.485-80.963 μg·mL-1. Conclusion: The developed method is simple, rapid and accurate, which provides a more comprehensive scientific basis for the quality evaluation of Kechuan mixture.

【基金】 常州医院协会-常州四药医院药学科研基金CJ20229003
  • 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2023年12期
  • 【分类号】O657.63;R286.0
  • 【下载频次】66
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