固相萃取净化-超高效液相色谱串联四级杆质谱检测鸡蛋及蛋制品中氯霉素和氟苯尼考药物残留

Simultaneous determination of chloramphenicol and florfenicol residues in eggs and egg products by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry

目的建立了鸡蛋、蛋制品中氯霉素和氟苯尼考的固相萃取/超高效液相色谱-串联质谱(LC-MS/MS)同时测定方法。方法样品中的目标化合物经1%三氯乙酸-乙腈提取,提取液经HLB固相萃取柱净化,氮气浓缩后用10%乙腈复溶,经过0.22μm尼龙滤膜过滤,采用WatersACQUITYUPLCBEHC18(2.1mm×50mm,1.7μm)色谱柱分离,超高效液相色谱-串联四级杆质谱测定。结果氯霉素和氟苯尼考在线性范围内有良好的线性关系,其相关系数(r≥0.9997),鸡蛋和蛋制品中氯霉素、氟苯尼考的检出限为0.05μg/kg,3个浓度水平的加标回收率为87.3%~97.3%,相对标准偏差(RSD)为4.3%~9.2%。结论该方法灵敏度高、操作简单、结果准确,适用于鸡蛋和蛋制品中氯霉素、氟苯尼考的同时快速测定。采用本检测方法对市售的20份鲜蛋样品进行检测,发现一例氟苯尼考阳性样品,结果显示鲜蛋中含有一定量的氯霉素类药物残留。

Objective Develop a method for detection of chloramphenicol,florfenicol in eggs and egg products by solid phase extraction - ultra performance liquid chromatography tandem mass spectrometry( UPLC - MS /MS) . Methods The compounds were extracted by 1% TFA - acetonitrile and cleaned up with HLB SPE column; after dried to dryness under nitrogen and dissolved by 10% acetonitrile,the solution went through 0.22 μm syringe filter,and chromatographic separation was performed on a Waters ACQUITY UPLC BEH C18 ( 2.1 × 50 mm,1.7 μm) column and detected by UPLC - tandem mass spectrometry. Results Chloramphenicol and florfenicol had good linear relationship with correlation coefficients(r) not less than 0.999 7, the limits of detection(LOD) for chloramphenicol and florfenicol were 0.05 μg /kg,the recovery rates at low,middle and high spiked levels were within 87.3 % - 97.3%,and the relative standard deviations were within 4.3% - 9.2%. Conclusion The method is of high sensitivity,simplicity,accuracy,and is suitable for the determination of chloramphenicol and florfenicol in eggs and egg products. In this test,20 samples of fresh eggs sold in the market were tested,and fluphenicol was found in a sample. The results showed that there was a certain amount of chloramphenicol residue in fresh eggs.