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
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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-5 ms capillary chromatographic column(30m × 0.25 mm,0.25 μm) 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 0.1-100.0 μg/m L,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 40.28 μg/g. The content in oviductus ranae,zaocys,and hydrophiswas 4.45,2.84,and 10.43 μg/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.
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-5 ms capillary chromatographic column(30m × 0.25 mm,0.25 μm) 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 0.1-100.0 μg/m L,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 40.28 μg/g. The content in oviductus ranae,zaocys,and hydrophiswas 4.45,2.84,and 10.43 μg/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.
引文
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[15]蒋璐,汪国威,李扬,等.海蛇风湿胶囊抗风湿作用的药效研究[J].中药新药与临床药理,2017,28(3):310-313.DOI:10.19378/j.issn.1003-9783.2017.03.010.
[16]周烨,易蔚.蛤蚧的药理作用及其治疗哮喘的作用机制研究综述[J].广西中医药大学学报,2011,14(4):79-80.DOI:10.3969/j.issn.1008-7486.2011.04.047.
[17]南北朝雷敩.雷公炮炙论[M].上海:中医学院出版社,1986:74-75.
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[19]胡绍兰.尾全蛤蚧与无尾蛤蚧体活性比较[J].北京中医,1996,5:37-38.
[2]LAUNAY M,POTIN D,MAILLET M,et al.Hydantoin compounds useful as anti-inflammatory agents[P].US,2002143035.2002-10-03.
[3]LU HB,KONG DJ,WU B,et al.Synthesis and evaluation of anti-inflammatory and antitussive activity of hydantoinderivatives[J].Lett Drug Des Disc,2012,9(6):638-642.DOI:10.2174/157018012800673092.
[4]高利娜,杨爽,刘俊亭,等.5-羟基-1-甲基海因对百草枯所致大鼠肾毒性防护作用的实验研究[J].中华危重病急救医学,2015,27(4):246-249.DOI:10.3760/cma.j.issn.2095-4352.2015.04.004.
[5]韩冬,董雪莲,邱智东.1-甲基海因对哮喘大鼠模型的平喘作用及其机制[J].吉林大学学报(医学版),2014,40(3):543-548.DOI:10.13481/j.1671-587x.20140316.
[6]罗海燕,雷羽,熊亮,等.青环海蛇中有效物质1-甲基海因的含量测定[J].时珍国医国药,2010,21(4):882-883.DOI:10.3969/j.issn.1008-0805.2010.04.055.
[7]张嵩,王维宁,陈芳芳,等.蛤蟆油与类似品和伪品的质量评价[J].沈阳药科大学学报,2012,29(12):951-958.DOI:10.14066/j.cnki.cn21-1349/r.2012.12.008.
[8]高竹青,刘俊亭,王春媛,等.对中国药典用1-甲基海因鉴别蛤蟆油方法的商榷[J].中南药学,2013,11(8):608-610.DOI:10.7539/j.issn.1672-981.2013.08.014.
[9]WYSS M,KADDURAHDAOUK R.Creatine and creatinine metabolism[J].Physiol Rev,2000,80(3):1107.
[10]GOODNOW R A,KANG L.Hydantoin-containing glucokinase activators[P].CH,CN1427838.2003-07-02.
[11]陈冰,王诗涵,徐阳,等.HPLC法测定脱脂林蛙油胶囊中1-甲基海因的含量[J].黑龙江畜牧兽医,2014,5:196-197.
[12]王永生,张辉,林喆,等.RP-HPLC测定蛤蟆油中1-甲基海因的含量[J].中国药学杂志,2008,2:146-148.DOI:10.3321/j.issn:1001-2494.2008.02.020.
[13]杨士慧,赵雨,张梅,等.蛤蟆油非水溶性成分酶解物药理活性研究[J].食品科技,2012,37(4):44-47.DOI:10.13684/j.cnki.spkj.2012.04.006.
[14]顾剑萍,林乾良.乌梢蛇的药理研究初报[J].中国现代应用药学,1986,3(4):4-8.
[15]蒋璐,汪国威,李扬,等.海蛇风湿胶囊抗风湿作用的药效研究[J].中药新药与临床药理,2017,28(3):310-313.DOI:10.19378/j.issn.1003-9783.2017.03.010.
[16]周烨,易蔚.蛤蚧的药理作用及其治疗哮喘的作用机制研究综述[J].广西中医药大学学报,2011,14(4):79-80.DOI:10.3969/j.issn.1008-7486.2011.04.047.
[17]南北朝雷敩.雷公炮炙论[M].上海:中医学院出版社,1986:74-75.
[18]商壁.岭表录异校补[M].南宁:广西民族出版社,1988:168.
[19]胡绍兰.尾全蛤蚧与无尾蛤蚧体活性比较[J].北京中医,1996,5:37-38.