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

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 %.