改良的QuEChERS与超高效液相色谱三重四极杆质谱法检测动物源性食品中胺苯醇类药物残留

目的建立改良的QuEChERS与超高效液相色谱三重四极杆质谱法(HPLC-MS/MS)检测动物源性食品中胺苯醇类药物的检测方法。方法样品经改进的QuEChERS方法提取净化,以氨化乙腈为提取剂,正己烷、乙二胺-N-丙基硅烷(PSA)净化粉、十八烷基硅烷键合硅胶(C₁₈)净化粉净化,Waters ACQUITY UPLC BEH C₁₈(2.1 mm×100 mm,1.7μm)柱色谱柱分离,超高效液相色谱三重四极杆质谱仪检测,外标法定量分析。结果采用本法测定,氯霉素、氟苯尼考胺、氟苯尼考和甲砜霉素得到很好的分离,在一定范围内呈现良好的线性关系。氯霉素的检出限为0.04μg/kg,氟苯尼考胺的检出限为2.0μg/kg,氟苯尼考和甲砜霉素的检出限为0.4μg/kg。样品的加标回收率为77.28%~104.5%,RSD在3.02%~6.49%。结论该方法实现了4种胺苯醇类药物残留的自动化、快速、高灵敏度和高稳定性分析,能够满足目前动物源性食品中胺苯醇类药物残留的检测限量的要求。

Residual determination of fenicol antibiotics in animal derived foods by modified QuEChERS combined with ultra performance liquid chromatography-triple quadrupole mass spectrometry

Objective A modified QuEChERS combined with ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS) method was established for the determination of fenicol antibiotics residual in animal derived foods. Methods Sample was extracted and purified by modified QuEChERS method;with ammoniation acetonitrile as extraction agent,N-hexane,ethylenediamine-n-propylsilane(PSA) purification powder,octadecyl silane bonded silica gel(C₁₈) purification powder were used for purification;Waters ACQUITY UPLC BEH C₁₈(2. 1 mm × 100 mm,1. 7 μm) column was used for separation;ultra-performance liquid chromatography triple quadrupole mass spectrometry was used for determination,and external standard method was used for quantitative analysis. Results By this method,chloramphenicol,florfenicol,florfenicol and sulfoxamycin were well separated and showed a good linear relationship in a certain range. The detection limits of chloramphenicol was 0. 04 μg/kg,the detection limit of florfenicol was 2. 0 μg/kg,and the detection limits of florfenicol and sulfoxamycin were 0. 4 μg/kg. The recoveries of the spiked samples were within 77. 28%-104. 5%,with RSDs of 3. 02%-6. 49%. Conclusion The method achieved automatic,rapid,high sensitivity and high stability analysis of four aminophenol residues,which can meet the current requirements of the detection limit of aminophenol residues in animal-derived food.