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目的建立基质固相分散-超高效液相色谱串联质谱法(UPLC-MS/MS)测定鸡肉中氯霉素(CAP)残留的测定方法。方法以氘代氯霉素(d5-CAP)为同位素内标,样品采用C18填料基质固相分散提取,正己烷淋洗,乙腈/水(V/V,50∶50)洗脱,洗脱液经乙酸乙酯萃取,氮气吹干后流动相定容待测。CAP在ACQUITY BEH C18色谱柱中分离,以水-甲醇做流动相梯度洗脱,以负离子多反应监测模式、同位素内标法定量。结果 CAP的检出限为0.01μg/kg,样品分别加标0.5μg/kg、10μg/kg和50μg/kg,加标回收率为85.0%~97.3%,相对标准偏差为5.4%~6.8%。结论本法具有非常高的选择性、灵敏度和准确度,完全能满足鸡肉中痕量氯霉素类药物残留的高灵敏分析。
OBJECTIVE To establish a method for the determination of chloramphenicol (CAP) residues in chicken by matrix solid phase dispersion-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The deuterated chloramphenicol (d5-CAP) was used as the internal standard of the isotope. The samples were solid-phase dispersed with C18 filler, eluted with n-hexane and eluted with acetonitrile / water (50:50 V / V) Extract with ethyl acetate and dry to dryness with nitrogen. CAP was separated on an ACQUITY BEH C18 column and eluted with a mobile phase of water-methanol. The CAP was monitored by anion-multiple reaction monitoring and isotope internal standard method. Results The detection limit of CAP was 0.01 μg / kg. The spiked samples were spiked with 0.5 μg / kg, 10 μg / kg and 50 μg / kg respectively. The recoveries were 85.0% -97.3% with relative standard deviations of 5.4% -6.8%. Conclusion This method has a very high selectivity, sensitivity and accuracy, fully meet the high sensitivity of trace chloramphenicol residues in chicken meat.