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作 者:张诚贤 吴芳媛 陈褚建 王新财 ZHANG Cheng-xian;WU Fang-yuan;CHEN Chu-jian;WAGN Xin-cai(Huzhou Institute for Food and Drug Control,Huzhou 313000,China)
出 处:《药物分析杂志》2021年第6期1064-1071,共8页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定木香顺气丸中木香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚、甘草酸、甘草苷、橙皮苷、柚皮苷、新橙皮苷、辛弗林10个成分的含量。方法:采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸乙腈溶液-0.1%甲酸水溶液,梯度洗脱,流速为0.3 mL·min^(-1),柱温为35℃,采用电喷雾离子源(ESI),正负离子同时扫描,多反应监测模式(MRM)对10个成分进行检测。结果:10个成分在测定的质量浓度范围内线性关系良好,相关系数(r)均大于0.995,平均回收率为92.8%~106.8%,RSD为1.6%~4.6%。6批木香顺气丸中木香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚、甘草酸、甘草苷、橙皮苷、柚皮苷、新橙皮苷和辛弗林的含量范围分别为0.467~0.923、1.276~2.127、0.748~4.665、2.081~4.791、0.887~1.012、0.234~0.422、14.892~23.516、3.539~6.799、2.652~5.072和0.259~0.570 mg·g^(-1)。结论:所建立的方法快速、准确,适用于木香顺气丸中木香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚、甘草酸、甘草苷、橙皮苷、柚皮苷、新橙皮苷和辛弗林10个成分的含量测定,为木香顺气丸多组分质量控制提供参考。Objective:To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for simultaneous determination of costunolide,dehydrocostus lactone,honokiol,magnolol,glycyrrhizic acid,liquiritin,hesperidin,naringin,neohesperidin and synephrine in Muxiang Shunqi pills.Methods:The components were separated on Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7μm)with 0.1%formic acid acetonitrile solution and 0.1%formic acid aqueous solution as the mobile phase by gradient elution.The flow rate was 0.3 mL·min^(-1).The column temperature was set at 35℃.The detection was carried out by electrospray ionization(ESI)in positive and negative modes.Multiple reaction monitoring(MRM)mode was used for quantitative analysis.Results:The linear relationships of ten components were good in corresponding concentrations with correlation coefficients(r)grenter 0.995.The average recoveries of ten components were 92.8%-106.8%with RSDs within 1.6%-4.6%.The contents of costunolide,dehydrocostus lactone,honokiol,magnolol,glycyrrhizic acid,liquiritin,hesperidin,naringin,neohesperidin and synephrine in Muxiang Shunqi pills were 0.467-0.923,1.276-2.127,0.748-4.665,2.081-4.791,0.887-1.012,0.234-0.422,14.892-23.516,3.539-6.799,2.652-5.072 and 0.259-0.570 mg·g^(-1),respectively.Conclusion:The method is rapid,accurate and suitable for simultaneous determination of costunolide,dehydrocostus lactone,honokiol,magnolol,glycyrrhizic acid,liquiritin,hesperidin,naringin,neohesperidin and synephrine in Muxiang Shunqi pills.The method can provide reference for the quality control of Muxiang Shunqi pills.
关 键 词:木香顺气丸 木香烃内酯 去氢木香内酯 和厚朴酚 厚朴酚 甘草酸 甘草苷 橙皮苷 柚皮苷 新橙皮苷 辛弗林 含量测定 超高效液相色谱-串联质谱
分 类 号:R917[医药卫生—药物分析学]
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