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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0.1 ng/g0、.2 ng/g和0.5 ng/g,平均回收率为89.9%~98.4%,相对标准偏差(RSD)均小于8.2%。
The residues of chloramphenicol, thiamphenicol and florfenicol in royal jelly were simultaneously determined by HPLC-MS / MS. Samples were added to the negative honey and water homogenized, extracted with ethyl acetate, concentrated by evaporation, C18 SPE purification. After HPLC separation, tandem mass spectrometry was used for qualitative and quantitative analysis by electrospray ionization multiple reaction monitoring (MRM). Through the optimization of solid-phase extraction conditions, greatly reducing the matrix interference. The detection limits of chloramphenicol, florfenicol and thiamphenicol were 0.1 ng / g0, 0.2 ng / g and 0.5 ng / g, respectively. The average recoveries were 89.9% ~ 98.4%. The relative standard deviations RSD) were less than 8.2%.