固相萃取-高效液相色谱法测定全血中克林沙星  

Determination of clinafloxacin in whole blood by high-performance liquid chromatography coupled with fluorescence detection

作　　者：陈琦君[1] 金米聪[2] 

机构地区：[1]浙江省宁波市微循环与莨菪类药研究所,浙江宁波315010 [2]浙江省宁波市疾病预防控制中心,浙江宁波315010

出　　处：《中国卫生检验杂志》2009年第10期2267-2269,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立一种灵敏、可靠的全血中克林沙星的固相萃取高效液相色谱荧光检测方法。方法：样品经磷酸盐缓冲液提取后用Oasis MAX小柱净化,采用乙腈-0.2%甲酸（30：70,v/v）为流动相,在Cloversil-C18柱（150 mm×3.0 mm,5μm）上进行分离,荧光法检测,以环丙沙星为内标进行定量,荧光检测波长为λex290 nm和λem490 nm。结果：全血中克林沙星含量在5.0-1000.0μg/L范围内呈良好线性,方法回收率在87.0%-95.2%之间,RSD〈6.0%,其定量检出限为5.0μg/L。结论：本方法简便、灵敏、干扰少、特异性好,能满足全血中克林沙星的临床药物残留的检测要求。Objective：To set up a sensitive and accurate method for the determination of clinafloxacin in whole blood by high -performance liquid chromatography with fluorescence detection. Methods：After clinafloxaein in whole blood was extracted by phosphate buffer, the sample was cleaned with solid - phase extraction （SPE） using Waters Oasis MAX cartridges. The separa- tion was performed on a Cloversil -C18 column（ 150 mm × 3. 0 mm, 5μm）using the mobile phase consisting of CH3 CN- 0.2% HCOOH （30：70, v/v）. Detection was carried out with a fluorescence detector at λex 290 nm and hem 490 nm using eiprofloxacin as an internal standard. Results：Calibration curve was linear within the range of 5.0 - 1000. 0 μg/L, and the extraction recoveries were from 87.0% to 95.2%, the RSD were less than 6.0%. The limit of quantification was 5.0 μg/L Conclusion： This method is simple, sensitive and of little interferential for the determination of elinafloxaein in whole blood.

关 键 词：高效液相色谱 荧光检测 全血 克林沙星 

分 类 号：O657.72[理学—分析化学]