UPLC-MS/MS法同时定量测定补中益气丸中的15种化合物

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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Rb_1、人参皂苷Rb_2、人参皂苷Rd、人参皂苷Rg_1、甘草酸和柴胡皂苷a的含量。方法:采用Zorbax Eclipse Plus C_(18)色谱柱(100 mm×2.1 mm,1.8μm);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,r~2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0.187~3.076μg·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。 OBJECTIVE: To establish a method for the simultaneous determination of liquiritin, naringin, hesperidin, neohesperidin, liquiritigenin, hesperetin, naringenin, ciliarin, astragaloside, Ginsenoside Rb - 1, ginsenoside Rb - 2, ginsenoside Rd, ginsenoside Rg - 1, glycyrrhizin and saikosaponin a. METHODS: Zorbax Eclipse Plus C_ (18) column (100 mm × 2.1 mm, 1.8 μm) was used as the mobile phase. The mobile phase consisted of 0.1% formic acid in acetonitrile and 0.1% formic acid and eluted with gradient elution. (ESI ~ -), quantitative analysis using multiple reaction detection mode (MRM). Results: The linear correlations were found between the two compounds in the corresponding mass concentration range. The r ~ 2 values ​​ranged from 0.992 to 0.998. The RSDs of the 15 compounds at low and high concentrations ranged from 1.2% to 4.56% and from 1.6% to 7.4% The average recoveries of 15 compounds ranged from 95.8% to 104.3%, and the corresponding RSD ranged from 2.4% to 8.7%. The average contents of the 15 components in the actual samples ranged from 0.187 to 3.076 μg · pill -1 . Conclusion: The analysis is completed in one step, which reduces the cost of analysis. Therefore, the method is simple, sensitive and has high throughput. It is a reliable method to detect TCM preparation of Buzhong Yiqi Pills.
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