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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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UPLC-MS/MS法同时定量测定补中益气丸中的15种化合物

UPLC-MS/MS method for simultaneous determination of 15 components in Buzhong Yiqi pills

作者(英文):
分类号:R917
出版年·卷·期(页码):2017,37 (7):1228-1233
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立UPLC-MS 法同时测定补中益气丸中甘草苷、柚皮苷、橙皮苷、新橙皮苷、甘草素、橙皮素、柚皮素、升麻素、黄芪甲苷、人参皂苷 Rb1、人参皂苷 Rb2、人参皂苷 Rd、人参皂苷 Rg1、甘草酸和柴胡皂苷 a 的含量。方法:采用Zorbax Eclipse Plus C18色谱柱(100 mm×2.1 mm,1.8 μm);流动相为0.1%甲酸乙腈溶液-0.1%甲酸溶液,梯度洗脱;质谱离子化方式为负源电喷雾(ESI-),定量分析采用多反应离子检测模式(MRM)。结果:各化合物在相应质量浓度范围内呈良好的线性关系,r2值为0.992~0.998;15种化合物低高浓度下的精密度RSD 分别在1.2%~4.56%和1.6%~7.4%之间; 15种化合物的平均加样回收率为95.8%~104.3%,相应的RSD在2.4%~8.7%间;实际样品中15种成分的平均含量在0.187~3.076 μg·丸-1结论:分析一步完成,降低了分析成本,因此该方法简便、高灵敏度、高通量,是检测补中益气丸中药制剂的可靠方法。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a UPLC-MS method for simultaneous determination of liquiritin, naringin, hesperidin, neohesperidin, liquiritigenin, hesperetin, naringenin, cimifugin, astragalosideIV, ginsenoside Rb1, ginsenoside Rb2, ginsenoside Rd, ginsenoside Rg1, glycyrrhizic acid, saikosaponin in Buzhong Yiqi pills.Methods: Agilent Zorbax Eclipse Plus C18(100 mm×2.1 mm, 1.8 μm)column was used. The gradient mobile phase consisted of water and acetonitrile both containing 0.1% formic acid. Mass spectrometer was operated using electrospray ionization(ESI-)source in the negative ion mode for detection. Mass data acquisition was done with multiple reaction monitoring(MRM). Results: Full validation of the assay was implemented. Excellent linear calibration curves were obtained over the tested concentration ranges(r2, 0.992-0.998). Intra-and inter-day precisions(RSD)of low and high quality controls were 1.2%-4.6% and 1.6%-7.4%, respectively. The mean extraction recoveries were all between 95.8% and 104.3%, and the RSD values were 2.4%-8.7%. In the analysis of commercial samples, the mean contents of the tested analytes were 0.187-3.076 μg per pill. Conclusion: This method significantly reduces the analysis cost. This new, reliable and high throughput method is beneficial for quantification assays of multiply components in Buzhong Yiqi pills.

-----参考文献:---------------------------------------------------------------------------------------

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