CAJ | 학술논문

目的：建立猪肉中22种磺胺类兽药残留的定性定量分析方法。方法采用固相萃取技术处理样品,通过高效液相色谱-四极杆-飞行时间质谱法对猪肉中的22种磺胺类药物进行分离和检测,并对其进行方法学验证,考察方法检测限、精密度、回收率等指标。建立磺胺类药物的精确相对分子质量数据库,并通过碎片离子的精确质量数推测碎片结构。结果在最低定量限到150μg/kg范围内,标准曲线相关性良好(r≥0.99),所测定的22种化合物检测限为0.1~5μg/kg,化合物回收率在81.1%~118.0%之间,精密度在1.9%~13.6%(n=5)之间。建立了磺胺类共22种化合物的精确相对分子质量数据库。结论建立的方法准确、快速、灵敏度高,结合精确相对分子质量数据库,可应用于实际案例中磺胺类兽药残留的快速分析。
목적：건립저육중22충광알류수약잔류적정성정량분석방법。방법채용고상췌취기술처리양품,통과고효액상색보-사겁간-비행시간질보법대저육중적22충광알류약물진행분리화검측,병대기진행방법학험증,고찰방법검측한、정밀도、회수솔등지표。건립광알류약물적정학상대분자질량수거고,병통과쇄편리자적정학질량수추측쇄편결구。결과재최저정량한도150μg/kg범위내,표준곡선상관성량호(r≥0.99),소측정적22충화합물검측한위0.1~5μg/kg,화합물회수솔재81.1%~118.0%지간,정밀도재1.9%~13.6%(n=5)지간。건립료광알류공22충화합물적정학상대분자질량수거고。결론건립적방법준학、쾌속、령민도고,결합정학상대분자질량수거고,가응용우실제안례중광알류수약잔류적쾌속분석。
Objective To establish a novel analytical method for the analysis on 22 sulfonamides (SAs) in pork by using high performance liquid chromatography-Q-time of fight mass spectrometry (HPLC-Q-TOF MS). Methods The analytes were extracted from the samples using acetonitrile. After separeted on C18 SPE column, samples were analyzed by HPLC-Q-TOF MS using an electrospray interface in positive ionisation mode. An accurate mass database was established for 22 SAs, and the structures of product ions were inferred by their accurate masses. Results The regression coefficients (r) for the calibration curves (LOQ~150 μg/kg) were ≥ 0.99, the LODs for 22 validated compounds were ranged from 0.1~5 μg/kg, and the recoveries were in the range of 81.1%~118.0%, and the relative standard deviations (RSD) were ranged from 1.9% to 13.6% (n=5). Conclusion The results indicated that this method is simple, rapid, sensitive and suitable for the determination of sulfonamides in pork.