摘要
目的基于LC-MS/MS测定复方苦参汤中苦参碱、氧化槐果碱、氧化苦参碱的含量。方法采用LC-MS/MS(Agilent 1260液相色谱仪,AB SCIEX 4000QTRAP三重四级杆质谱仪),Agilent 5 TC-C18(2)(250mm×4.6mm,5μm)色谱柱,流动相为甲醇-水,梯度洗脱,流速400μL/min,进样量5μL,柱温30℃;离子源为ESI源,采用正离子模式进行检测,检测离子对质荷比为:苦参碱(249.2/148.3)、氧化槐果碱(262.9/136.1)、氧化苦参碱(265.3/136.1)。结果苦参碱、氧化槐果碱、氧化苦参碱的线性关系良好(r>0.995),平均加样回收率分别为99.7%(RSD=3.4%)、102.1%(RSD=3.1%)、100.8%(RSD=2.9%),10批样品中苦参碱、氧化槐果碱、氧化苦参碱含量分别在0.4475～0.5229 mg/mL、0.0564～0.0812mg/mL、0.1512～0.2142mg/mL范围内。结论该法简便、快捷、可行性强,可用于测定复方苦参汤中苦参碱、氧化苦参碱、氧化槐果碱含量。
Objective To determine matrine, sophocarpidine and oxymatrine in Fufang Kushen decoction based on LC- MS/MS. Methods Using LC-MS/MS （Agilent 1260 liquid chromatography, AB SCIEX 4000QTRAP triple quadrupole mass spectrometer）, Agilent 5 TC-C 18（ 2 ）（250mm×4.6mm, 5μm） column, the mobile phase consisted of methanol and water, gradient elution, flow rate of 400 μL/min, sample volume 5μL, the column temperature was 30℃; the ion source was ESI , and the positive ion mode was used to detect the alkaloids; the detection ratios for ion confrontation： matrine（249.2/148.3）, sophocarpidine （262.9/136.1）, oxymatrine（265.3/136.1）. Results The linear relationship between matrine, sophocarpidine and oxymatrine was good （r〉0.995）, the average recovery rates were 99.7% （RSD=3.4%）, 102.1%（RSD=3.1%）, 100.8%（RSD=2.9%）; 10 batches of samples of matrine sophocarpidine and oxymatrine content were 0.4475-0.5229mg/mL, 0.0564-0.0812mg/mL, 0.1512-0.2142mg/mL range. Conclusion The method is simple, fast and feasible. It can be used for the determination of matrine, sophocarpidine and oxymatrine in Fufang Kushen decoction.
作者
洪宗超
吴和珍
杨艳芳
柳阳
范恒
段雪云
HONG Zongchao;WU Hezhen;YANG Yanfang;LIU Yang;FAN Heng;DUAN Xueyun(Hubei University of Chinese Medicine, Wuhan 430065;Department of Integrated Chinese and Western Medicine, Union Hospital, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430022;Hubei Provincial Hospital of Traditional Chinese Medicine, Wuhan 430061)
出处
《湖北中医药大学学报》
2018年第2期39-42,共4页
Journal of Hubei University of Chinese Medicine
基金
国家自然科学基金面上项目(项目编号:81573784)
中国中医科学院中医基础理论研究所自主选题项目(项目编号:YZ-1605)
