高效液相色谱-串联质谱法同时测定蜂王浆中氯霉素、甲砜霉素和氟甲砜霉素残留  

Simultaneous Determination of Residues of Chloramphenicol,Thiamphenicol and Florfenicol in Royal Jelly by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：王鹏[1] 胡小钟 林雁飞 罗静 高晓丹[1] 郭少飞[1] 荆涛[1] 梅素容[1] 周宜开[1] 

机构地区：[1]华中科技大学同济医学院公共卫生学院教育部环境与健康重点实验室,武汉430030 [2]湖北出入境检验检疫局,武汉430022

出　　处：《分析科学学报》2007年第5期527-531,共5页Journal of Analytical Science

基　　金：国家自然科学基金(No.20407009);湖北省自然科学基金(No.2003ABA060)

摘　　要：采用高效液相色谱-串联质谱（HPLC—MS／MS）法同时测定了蜂王浆中氯霉素、甲砜霉素和氟甲砜霉素残留。样品加入阴性蜂蜜和水均质后，采用乙酸乙酯提取，蒸发浓缩，C18固相萃取净化。HPLC分离后，串联质谱法以电喷雾负离子多反应监测方式（MRM）进行定性定量分析。通过对固相萃取条件的优化，大大减小了基质的干扰。氯霉素、氟甲砜霉素和甲砜霉素的检出限分别为0．1ng／g、0．2ng／g和0．5ng／g，平均回收率为89．9%～98．4％，相对标准偏差（RSD）均小于8．2％。A method was presented for simultaneous determination of residues of chloramphenicol （CAP）, thiamphenicol （TAP） and florfenicol （FF） in royal jelly by using high performance liquid chromatography tandem mass spectrometry （LC-MS/MS）. After a preliminary homogenization with negative honey and water, samples were extracted with ethyl acetate, and evaporated to dryness; then, the clean up was carried out on a C18 SPE cartridge. In order to decrease the matrix interference, the conditions of solid phase extraction were optimized. After reversed-phase HPLC separation, identification and quantification were performed using multiple reaction monitoring （MRM） and electrospray ionization in negative mode. The detection limits for CAP,FF and TAP were 0.1 ng.g^-1 , 0.2 ng.g^-1 and 0.5 ng.g^-1, respectively with the average recoveries of 89.9%-98.4% and the RSD less than 8.2 %.

关 键 词：氯霉素 蜂王浆 固相萃取 高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]