液相色谱-串联质谱法测定血清和尿液中硝基咪唑类药物残留  

Residue Determination of Nitroimidazoles in Sera and Urine by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：张金玲[1] 郭礼强[1] 孙军[1] 吴翠玲[2] 

机构地区：[1]潍坊出入境检验检疫局,山东潍坊261041 [2]安捷伦科技(中国)有限公司,北京100102

出　　处：《动物医学进展》2017年第7期56-61,共6页Progress In Veterinary Medicine

基　　金：山东出入境检验检疫局科研基金项目(SK201349);潍坊市2015年科学技术发展计划项目(2015ZJ1101)

摘　　要：为建立血清和尿液中甲硝唑、羟基甲硝唑、二甲硝咪唑和羟基二甲硝咪唑的高效液相色谱-串联质谱(HPLC-MS/MS)快速测定方法,样品用乙酸乙酯提取,经PCX固相萃取柱净化,Eclipse Plus C18色谱柱(3.0mm×100mm,1.8μm)分离,进行HPLC-MS/MS分析。结果表明,甲硝唑、羟基甲硝唑、二甲硝咪唑及羟基二甲硝咪唑在0.20μg/L^50μg/L范围呈良好线性,线性相关系数均大于0.995,检出限为0.20μg/L,定量下限为0.50μg/L。样品在定量下限1、2、10倍3个加标水平下的平均回收率为89.3%~108.2%,相对标准偏差(RSD)为2.63%~10.0%。该方法灵敏、简便、准确,可用于血清和尿液中硝基咪唑类药物的检测分析。A method for the determination of metronidazole, hydroxy metronidazole, dimetridazole and hydroxy dimetridazole in sera and urine by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was established.The target compounds were purified with solid phase extraction column of PCX after extraction by ethyl acetate.Then the samples was separated by an Eclipse Plus C18 column（3.0 mm×100 mm,1.8 μm）and analyzed by HPLC-MS/MS.The calibration curves were linear in the range of 0.2 μg/L-50μg/L for metronidazole, hydeoxy metronidazole, dimetridazole and hydeoxy dimetridazole with correlation coefficient （r） more than 0,995. The LOD was 0.2 μg/L and the LOQ was 0.5μg/L.The average recoveries （n=6） in feed samples at three spiked levels（1 times,2 times,10 times） ranged from 89.3%-108.2% with relative standard deviations （RSDs） of 2.63%-10.0%.The method was sensitive, convenient and accurate, and could satisfy the demand of detection and analysis of nitroimidazoles in serum and urine samples.

关 键 词：液相色谱-串联质谱 血清 尿液 残留分析 硝基咪唑 

分 类 号：S859.7[农业科学—临床兽医学]