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基于二维高效液相色谱的头孢哌酮血药浓度测定

Determination of cefoperazone plasma concentration by 2-dimensional high performance liquid chromatography
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摘要 目的建立二维高效液相色谱测定头孢哌酮血药浓度的方法,用于临床患者血液中头孢哌酮浓度的测定。方法样品去除蛋白后直接进样,分析柱为Aston C18色谱柱(4.6 mm×150 mm,5μm),萃取柱为Aston色谱柱(4.6 mm×25 mm,5μm)。流动相:第一维流动相为水(含20.0 mmol·L-1磷酸铵)∶乙腈∶甲醇=300∶100∶100(V/V/V),磷酸调pH至5.4;第二维流动相通过低压梯度四元泵自动配比,检测波长282 nm,参照波长232 nm,温度:40℃,进样量:200μL。结果头孢哌酮在2.03129.7μg·mL^-1与峰面积线性关系良好,R2=0.9999,定量限为2.03μg·mL^-1,绝对回收率为82.70%94.6%,日间日内RSD均小于7%。结论二维高效液相色谱法检测头孢哌酮血药浓度简单快速,准确稳定,灵敏度高,适用于头孢哌酮血药浓度日常监测。 Objective To establish a 2-dimensional high performance liquid chromatography(2 D-HPLC) method for the determination of cefoperazone plasma concentration. Methods The sample was injection to a column after eliminating the protein. The analytical column was Aston C18(4.6 mm×150 mm, 5 μm), and the extraction column was Aston(4.6 mm×25 mm, 5 μm). The first dimension of the mobile phase consisted of water(containing 20 mmol·L-1 ammonium phosphate)∶acetonitrile∶methanol = 300∶100∶100(V∶V∶V)(pH = 5.4). The second dimension of the mobile phase was automatic-mix by pump. The detection wavelength was 282 nm, the reference wavelength was 232 nm, the temperature was 40℃, and the injection volume was 200 μL. Results The calibration curve of cefoperazone showed good linearity at 2.03-129.7 μg·m L-1(R2= 0.9999), and the quantitation limit was 2.03 μg·mL^-1. The absolute recoveries were 82.70%-94.6%. The RSDs of intra-day and inter-day assays were less than 7%. Conclusion The 2 D-HPLC method for the determination of cefoperazone plasma concentration is not only simple and quick, but also accurate and stable, with high sensitivity suitable for the routine monitoring of cefoperazone plasma concentration.
作者 彭国茳 曹毅 王峰 李林 周建军 PENG Guo-jiang;CAO Ni;WANG Feng;LI Lin;ZHOU Jian-jun(Affiliated Hospital of Xiangnan Institute,Chenzhou Hunan 423000;Department of Pharmacy,Second Xiangya Hospital,Central South University,Changsha 410011;ANAX Instruments Company Limited,Changsha 410000;College of Pharmacy,Xiangnan University,Chenzhou Hunan 423000)
出处 《中南药学》 CAS 2019年第1期105-108,共4页 Central South Pharmacy
基金 省卫计委项目(No.B2016154) 湘南学院校级课题(No.2015XB16,2016XJ58).
关键词 二维高效液相色谱 头孢哌酮 血药浓度 2-dimensional high performance liquid chromatography cefoperazone plasma concentration
作者简介 彭国茳,男,药师,主要从事临床药学、药物分析研究,E-mail:pgjiang65@163.com;通讯作者:周建军,男,副主任药师,主要从事l临床药学研究,E-mail:934538571@qq.com.
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