HPLC-UV法同时检测犬血浆中异甘草酸镁及甘草次酸  被引量:3

Simultaneous measurement of magnesium isoglycyrrhizinate and glycyrrhetic acid in plasma of dog by HPLC

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作  者:刘苏怡[1] 王庆敏[1] 曹聪[1] 丁建花[1] 胡刚[1] 

机构地区:[1]南京医科大学药理学系

出  处:《中国临床药理学与治疗学》2006年第12期1395-1400,共6页Chinese Journal of Clinical Pharmacology and Therapeutics

摘  要:目的:建立同时检测犬血浆中异甘草酸镁(MGL)及甘草次酸(GA)的高效液相紫外检测法(HPLC-UV)。方法:采用HPLC-UV法,检测波长252nm,Kromasil ODS-1 C18色谱柱,柱温25℃.流动相:乙腈-0.1%二乙胺水溶液(pH4.60),二元梯度洗脱,流速1.0ml·min^-1,Millennium^32工作站采集数据,外标法计算血药浓度。结果:血浆中MGL、GA峰分离良好,内源性物质不干扰样品峰。最低定量浓度为0.2mg·L^-1,两者浓度范围在0.2~100mg·L^-1呈线性相关;相对回收率分别为94.3%~101.9%和96.4%~101.9%,绝对回收率分别为78.7%~87.0%和77.5%~87.7%,日内和日间变异均小于15.0%;血浆样品-20℃冰箱中冻存14d、冻融3次、室温放置10h均稳定,提取后样品4℃放置9h稳定。结论:本实验方法具有专属性,灵敏可靠,适用于MGL制剂给药后血药浓度的检测。AIM: To quantify magnesium isoglycyrrhizinate(MGL) and glycyrrhetic acid in the plasma of dog by develop a simple, rapid, sensitive high-perfomlance liquid chromatography ( HPLC-UV ) method. METHODS: HPLC-UV methods with wavelength 252 nm were used for the quantitation of MGL and GA in plasma. The concentration of MGL and GA were assayed on a Kromasil ODS-1 C18 column with the column temperature 25 ℃. The mobile phase was a gradient system with 0.1% diethylamine in water (pH 4.60) and acetonitrile at a flow rate of 1.0 ml·min^-1. RESULTS: There was a good linear response range of 0.2 - 2.5 mg·L^-1 and 2.5 - 100 mg· L^-1, while the limit of quantification was 0.2mg· L^-1. The relative recovery rate of MGL was 94.3 % -101.9%,GA%.4%- 101.9% (n=5);the absolute recovery rate was MGL 78.7% - 87.0%, GA 77.5 % - 87.7 % ( n= 5). The intra-day and inter-day variations were all less than 15% ( n= 5). The plasma samples preserved in refrigerator is stable at - 20 ℃ for 14 days, freeze thawing 3 times and at room temperature for 10 h without degradation. CONCLUSION: This method is shown to be specific, sensitive, reliable and suitable for the quantitative detemaination of magnesium isoglycynlaizinate following oral administration in biological sample.

关 键 词:异甘草酸镁 甘草次酸 高效液相紫外检测法 梯度洗脱 

分 类 号:R969.1[医药卫生—药理学]

 

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