基于液相质谱联用测定复方苦参汤中三种生物碱的含量  

Determination of Three Alkaloids in Fufang Kushen Decoction Based on LC-MS/MS

作　　者：洪宗超 吴和珍[1] 杨艳芳[1] 柳阳 范恒[2] 段雪云[3] 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)

机构地区：[1]湖北中医药大学,湖北武汉430065 [2]华中科技大学同济医学院附属协和医院中西医结合科,湖北武汉430022 [3]湖北省中医院,湖北武汉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)

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.

关 键 词：LC-MS/MS 复方苦参汤 苦参碱 氧化槐果碱 氧化苦参碱 含量测定 

分 类 号：R284.1[医药卫生—中药学]