多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量  

Determination of 8 Kinds of Cephalosporins in Aquatic Products by Multi-walled Carbon Nanotubes Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Mass Spectrometry

作　　者：顾蓓乔[1] 梅光明[1] 张小军[1] 何依娜[1] 严忠雍[1] 朱敬萍[1] 

机构地区：[1]浙江省海洋水产研究所,浙江省海水增养殖重点实验室,舟山316021

出　　处：《分析化学》2017年第3期381-388,共8页Chinese Journal of Analytical Chemistry

基　　金：浙江省科技厅计划项目(Nos.2016C32074;2016F30022)资助~~

摘　　要：建立了水产品可食部位中头孢哌酮、头孢喹肟、头孢洛宁、头孢唑啉、头孢匹林、头孢噻呋、头孢匹罗和头孢氨苄8种头孢菌素的超高效液相色谱-质谱测定法。样品经乙腈-水溶液提取、多壁碳纳米管固相萃取净化后,以Acquity Xselect CSH C_(18)柱为分离柱,用乙腈和0.1%甲酸溶液进行梯度洗脱,电喷雾正离子多反应模式监测。结果表明,8种头孢菌素均呈良好的线性关系(R^2≥0.995),定量限(S/N=10)在2~10μg/kg之间;在阴性样品采取梯度加标,添加回收率为67.3%~94.2%,RSD为3.3%~14%。本方法检测成本低、准确度高、精密度好,能够满足水产品中头孢菌素检测的要求。An ultra-high performance liquid chromatography-mass spectrometry （UPLC-MS/MS） method was developed for the determination of 8 kinds of cephalosporins, cefoperazone, cefquinome, cefalonium, cefazolin, cefapirin, Ceftiofur, cefpirome and cefalexin, in edible parts of aquatic products. The samples were extracted with acetonitrile-water and cleaned up by multi-walled carbon nanotubes （MWCNTs） SPE cartridge.All the target compounds were separated on all Acquity Xselecl CSH C18 column with gradient elution by using acetonitrile and 0.1% formic acid aqueous as eluent, and detected by UPLC-MS/MS under ESI＋ ionization and MRM mode. Under optimized conditions, this method had a good linearity （R2 ≥0. 995 ） and the limits of quantification were in the range of 2-10 μg/kg （S/N = 10）. The recoveries of the method for the target compounds spiked at three different levels were 67.3%-94.2% with the relative standard deviations （RSDs） of 3.3%-14%. The method had the characteristics of low cost, high accuracy and good precision, and could meet the requirements of cephalosporins determination.

关 键 词：多壁碳纳米管 超高效液相色谱-质谱法 水产品 头孢菌素 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]