动物药羊胆水质量标准研究
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摘要
目的建立羊胆水药材的质量标准。方法采用薄层色谱法对羊胆水进行定性鉴别。采用高效液相色谱(HPLC)法对羊胆水中胆酸含量进行测定,色谱柱为Phenomenex Luna-C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(45∶55),流速为1.0 mL/min,检测波长为192 nm,进样量为5μL,柱温为35℃。结果羊胆水药材的薄层色谱斑点清晰,与对照药材羊胆粉主斑点一致;总固体含量范围0.0461～0.0760 g/mL;胆酸在0.4225～6.7600 g/L范围内与峰面积线性关系良好(r=0.9995);专属性、精密度、稳定性均良好;平均加样回收率为98.58%,RSD为1.43%(n=9); 10批羊胆水药材中胆酸含量范围为7.537～19.660 g/L。结论该方法操作简单、准确、稳定、可靠,可为羊胆水的质量控制提供参考。
Objective To establish the quality standard of Fel Capra seu ovis.Methods TLC method was adopted to identify Fel Capra seu oris.HPLC method was used for content determination of cholic acid in Fel Capra seu ovis,the chromatographic column was Phenomenex Luna-C_(18) column(250 mm × 4.6 mm,5 μm),the mobile phase was acetonitrile-0.1% phosphoric acid solution(45 ∶55),the flow rate was 1.0 m L/min,the detection wavelength was 192 nm,the sample size was 5 μL,and the column temperature was 35 ℃.Results The TLC spots of Fel Capra seu ovis were clear and consistent with the main spots of the reference crude herb.The content of total solids was in the range of 0.0461-0.0760 g/m L.The cholic acid showed good linear relationship in the range of 0.4225-6.7600 g/L(r = 0.9995).The specificity,precision and stability were all good.The average recovery was 98.58% and RSD was 1.43%(n = 9).The content of cholic acid in 10 batches of Fel Capra seu ovis in the range of 7.537-19.660 g/L.Conclusion The method is simple,accurate,stable and reliable,which can provide reference for the quality control of Fel Capra seu ovis.
Objective To establish the quality standard of Fel Capra seu ovis.Methods TLC method was adopted to identify Fel Capra seu oris.HPLC method was used for content determination of cholic acid in Fel Capra seu ovis,the chromatographic column was Phenomenex Luna-C_(18) column(250 mm × 4.6 mm,5 μm),the mobile phase was acetonitrile-0.1% phosphoric acid solution(45 ∶55),the flow rate was 1.0 m L/min,the detection wavelength was 192 nm,the sample size was 5 μL,and the column temperature was 35 ℃.Results The TLC spots of Fel Capra seu ovis were clear and consistent with the main spots of the reference crude herb.The content of total solids was in the range of 0.0461-0.0760 g/m L.The cholic acid showed good linear relationship in the range of 0.4225-6.7600 g/L(r = 0.9995).The specificity,precision and stability were all good.The average recovery was 98.58% and RSD was 1.43%(n = 9).The content of cholic acid in 10 batches of Fel Capra seu ovis in the range of 7.537-19.660 g/L.Conclusion The method is simple,accurate,stable and reliable,which can provide reference for the quality control of Fel Capra seu ovis.
引文
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[2]江苏新医学院.中药大辞典(上下册)[M].上海:科学技术出版社,1977:962.
[3]高松.辽宁中药志(动物、矿物、海洋类)[M].沈阳:辽宁科学技术出版社,2015:294.
[4]贵州省药品监督管理局.贵州省中药材、民族药材质量标准[M].贵阳:贵州科技出版社,2003:196.
[5]赵文静,蒋蕾,旺建伟.羊胆汁抗急性炎症作用与PGE2含量变化相关的实验研究[J].中医药信息,2009,26(5):50-52.
[6]赵文静,蒋蕾,旺建伟.羊胆汁对炎症介质含量影响的实验研究[J].四川中医,2010,28(1):32-33.
[7]赵文静,蒋蕾,旺建伟.羊胆汁与其主要成分抗炎作用的比较研究[J].中医药学报,2009,37(4):20-22.
[8]冯玉龙.肺结核病羊胆疗法[M].上海:上海科学技术出版社,1959:1.
[9]郝丽莉,赵文静,王亚威.动物胆汁的药用研究[J].中国民族民间医药杂志,1999(5):279-280.
[10]王凯平,石朝周.动物胆汁药用研究的概况与展望[J].中国中医药科技,2000,7(5):350-352.
[11]黄有霖.福建省食品药品监督管理局.福建省中药材标准[M].福州:海风出版社,2006:103-104.
[12]邢世瑞.宁夏中药材标准[M].银川:宁夏人民出版社,1993:8-10.
[13]陈仁兴.高效液相色谱法及其在中药研究中的应用和展望[J].蛇志,2011,23(4):375-377.
[14]王一博,王春雨,曲范娜,等.高效液相色谱-电雾式检测器同时测定猪、牛、羊、熊胆粉中5种胆汁酸的含量[J].分析化学,2014,42(1):109-112.
[15]曹金山.胆酸的抗炎作用及对呼吸系统的药理作用和组织学影响[D].呼和浩特:内蒙古农业大学,2001.