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目的建立苍耳子复方颗粒剂中毒性成分苍术苷的快速高分离度液相色谱-串联质谱(RRLC-MS/MS)含量快速检测方法。方法将处理后的样品中加入内标氯霉素,运用超高效液相-质谱联用仪,采用多反应离子监测(MRM)在负离子检测模式下测定苍术苷的含量。结果苍术苷在0.505～505 ng.mL-1浓度范围内与峰面积积分值呈良好的线性关系(r=0.9993);平均回收率为95.38%,RSD=6.265%(n=6)。结论本研究所建立的含量测定方法快速、准确、稳定,可为苍耳子复方制剂中毒性成分苍术苷的检测提供快速准确的定量分析方法。
OBJECTIVE To establish a rapid and sensitive method for rapid determination of atractyloside in Xanthium Compound Granule by high performance liquid chromatography-tandem mass spectrometry (RRLC-MS / MS). Methods The internal standard chloramphenicol was added to the treated samples. The content of atractyloside was determined by the multi-reactive ion monitoring (MRM) in negative ion detection mode by using ultra-high performance liquid chromatography-mass spectrometry. Results The results showed that there was a good linear relationship between the concentrations of atractyloside and peak area in the range of 0.505 ~ 505 ng · mL-1 (r = 0.9993). The average recovery was 95.38% and the RSD was 6.265% (n = 6). Conclusion The method established in this study is rapid, accurate and stable and can provide a fast and accurate method for the quantitative determination of atractyloside in Xanthium Compound.