液相色谱-串联质谱法测定水产品中甲氧苄啶的残留  

Determination of trimethoprim residues in aquatic products by high performance liquid chromatography tandem mass spectrometry

作　　者：郑重莺 张海琪[1] 周燕[1] 周凡[1] 林静[1] 

机构地区：[1]浙江省水产质量检测中心,杭州310012

出　　处：《中国渔业质量与标准》2012年第2期89-93,共5页Chinese Fishery Quality and Standards

基　　金：浙江省重点科技创新团队项目(2010R50028)

摘　　要：建立甲氧苄啶液相色谱串联质谱(LC-MS/MS)的检测方法。方法:样品经乙腈提取后进行液相色谱-串联质谱分析。液相色谱柱为ODS-C3柱,乙腈和0.1%甲酸水溶液为流动相,梯度洗脱,流速200μL/min;质谱采用多反应检测扫描技术(Multireaction monitoring,MRM),甲氧苄啶采用正离子模式,监测的离子对为m/z291>m/z230.2,m/z291>m/z230.2。检测结果显示:甲氧苄啶的检出限为1.0μg/kg,线性范围为0～200ng/mL,回收率范围为81.7%～98.0%。结论:利用液相色谱串联质谱技术测定水产品中的甲氧苄啶残留的方法具有高选择性、高灵敏度、快速等特点,特别适合实验室大样品量的检测,具有实用性。The study aimed to establish a high performance liquid chromatography tandem mass spectrometry （HPLC -MS/MS） detection method of trimethoprim. Methods： Samples were extracted with acetonitrile for liquid chromatography - tandem mass spectrometry. Liquid column was ODS - C3 column, acetonitrile and 0.1% formic acid water as mobile phase, gradient elution, flow rate 200 μL/min; mass spectrometry using multiple reaction monitoring scanning technology （ multi reaction monitoring）, trimethoprim using positive ion mode, monitoring ion of the m/z 291 〉 m/z 230.2, m/z 291 〉 m/z 230.2. Results ： Trimethoprim detection limit was found to be 1.0 txg/kg, with the linear range of 0 -500 ng/mL, and recoveries was in the range between 81.7 to 98.0%. Conclusion： The use of liquid chromatography tandem mass spectrometry determination of aquatic products in the detection of trimethoprim residual was a fast detection method, which has high selectivity, sensitivity, and was especially suitable for the detection of large amount of laboratory samples, with practicability.

关 键 词：甲氧苄啶 水产品 液相色谱串联质谱 

分 类 号：O657.63[理学—分析化学]