基于气相色谱-质谱法的动物类中药材中1-甲基海因分布研究  

Gas Chromatography-mass Spectrometry Study of the Distribution of 1-Methylhydantoin in Medicinal Materials from Animals

作　　者：袁慧雅[1] 高利娜[1] 刘国杰 徐恩宇[1] 刘俊亭[1] YUAN Huiya;GAO Lina;LIU Guojie;XU Enyu;LIU Junting(Department of Toxicological Analysis,School of Forensic Medicine,China Medical University,Shenyang 110122,China;Department of Chemistry,School of Fundamental Sciences,China Medical University,Shenyang 110122,China)

机构地区：[1]中国医科大学法医学院毒物分析教研室,沈阳110122 [2]中国医科大学公共基础学院化学教研室,沈阳110122

出　　处：《中国医科大学学报》2018年第5期402-405,共4页Journal of China Medical University

基　　金：国家自然科学基金(81671864;81601644);辽宁省自然科学基金(20170541031)

摘　　要：目的 气相色谱-质谱法联合测定8种动物类中药材1-甲基海因的分布情况。方法 采用HP-5ms毛细管柱(30 m×0.25mm,0.25μm)。程序升温,初始柱温为60℃,保持1 min,以20℃/min升温至260℃。进样口温度为265℃,离子源温度为230℃。对蛤蚧各个解剖部位进行测定,并同时测定蛤蟆油、乌蛇、海蛇、地龙、全蝎、阿胶和紫河车中1-甲基海因含量。结果 1-甲基海因在0.1~100.0μg/m L浓度范围内线性关系良好(r=0.999 2),平均加样回收率为96.82%,相对标准差(RSD)为0.9%。蛤蚧头、脊椎、骨骼肌、四肢、皮肤和尾部含量分别为0.74、1.21、4.04、1.28、0.84、40.28μg/g;乌蛇和海蛇含量分别为2.84、10.43μg/g;蛤蟆油中含量为4.45μg/g。结论 气相色谱-质谱法能够准确测定动物类中药材中1-甲基海因含量;1-甲基海因为多种中药材共有成分,可能是蛤蚧、乌蛇、海蛇和蛤蟆油的共同药理活性基础物质之一。Objective To establish ahigh-performance liquid chromatography(HPLC)method for the determination ofthe distribution of 1-methylhydantoin(1-MH)in eight medicinal materials from Chinese animals.Methods The HP-5ms capillary chromatographic column(30 m×0.25 mm,0.25μm)was used.The oven temperature was initially set to 60℃for 1 min and then heated to 260℃at a rate of 20℃/min.The inlet temperature was 265℃and the ion source temperature was 230℃.Thematerials oviductusranae,zaocys,hydrophis,pheretima,scorpio,asinicoriicolla,and hominis placentawere analyzed.Results A good linear relationship was obtained in the range of 0.1-100.0μg/mL,with a correlation coefficient of r=0.999 2.The average recovery of the method was 96.82%(relative standard deviation:0.9%).1-MH was detected in the head,spine,skeletal muscle,limbs,skin,and tail of gecko at 0.74,1.21,4.04,1.28,0.84,and 40.28μg/g.The content in oviductus ranae,zaocys,and hydrophiswas 4.45,2.84,and 10.43μg/g,respectively.Conclusion This method can accurately determine the content of 1-MH in medicinal materials from animals.These results may demonstrate the common basis of the pharmacological activity of gecko,oviductusranae,zaocys,and hydrophis.

关 键 词：1-甲基海因 蛤蚧 蛤蟆油 气相色谱-质谱法 

分 类 号：R917[医药卫生—药物分析学]