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作 者:郭平[1] 李章万[1] 陈朝红[1] 邓尚平 唐尚国
机构地区:[1]华西医科大学药学院 [2]糖尿病胰岛素研究室,成都610041
出 处:《药学学报》1992年第6期452-455,共4页Acta Pharmaceutica Sinica
摘 要:采用HPLC柱切换技术,以Merck Lichroprep RP2(25~40μm)为预处理柱填料,以水为预处理流动相,以0.2mol/L乙酸-乙酸铵为净化清洗液,血浆直接进样,在线富集净化样品。血浆样品以0.2ml/min慢速转移通过预处理柱,净化回收率达80%。以ShimpackCLC-ODS为分析柱(15cm×6mm,ID),甲醇-异丙醇-0.2mol/L 乙酸铵(61:5:34)为分析流动相,310nm波长检测,外标法定量测定人体血浆中糖肾平的浓度。血浆样品仅需稀释后即可进样,净化富集样品操作简便,预处理柱可长期反复进样使用。血浆中最低检测浓度为30ng/ml,日内变异系数为2.0%~5.4%,日间变异系数为2.4%~2.7%,在浓度为60~2020ng/ml血浆范围内呈线性关系。An automated clean up and concentration method by column switchingis described for the assay of gliquidone, a hypoglycemic agent, in plasma. The systemuses Merck Lichroprep RP2 (25~40μm) as short precolumn packing material foron-line slean up and concentration. A Shimpack CLC-ODS (5μm) is used as analyti-cal column. Water is used as the pretreatment mobile phase and a mixture ofmethanol-isopropanol-0.2 mol/L ammonium acetate solution (61: 5: 34) isused as the analytical mobile phase. The plasma is diluted with a soluton of 0. 2 mol/Lacetic acid and injected directdly on the precolumn. The low speed of 0. 2 ml/min of pre-treatment mobile phase during transfer of plasma sample on the precolumn can get re-covery of 80.7%. The detection is at 310 nm and the detection limit is 30 ng/mlplasma. The procedure is simple and automatic.
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