摘要
目的建立一种超高效液相色谱-四极杆串联线性离子阱质谱技术测定乳制品中8种青霉素类抗生素（青霉素G、氨苄西林、青霉素V、阿莫西林、苯唑西林、萘夫西林、氯唑西林、双氯西林）及其相应的代谢产物青霉噻唑酸（青霉素G噻唑酸、氨苄青霉噻唑酸、青霉素V噻唑酸、羟氨苄青霉噻唑酸、苯唑青霉噻唑酸、乙氧萘青霉噻唑酸、氯唑青霉噻唑酸、双氯青霉噻唑酸）残留的方法,并对市售乳制品中青霉素及青霉噻唑酸残留情况进行调查。方法乳制品样品中青霉素及青霉噻唑酸采用纯水超声提取,经乙腈沉淀蛋白,正己烷液液萃取除去脂肪,用氮气吹至近干,用乙腈-水（10∶90,V/V）复溶后,经0.22μm微孔滤膜过滤,经超高效液相色谱C18柱（50 mm×2.1 mm,1.8μm）分离,选用乙腈-水（含0.1%甲酸）为流动相,梯度洗脱分离8种青霉素及相应青霉噻唑酸共16种组分;在优化的四极杆串联线性离子阱质谱条件下,采用ESI源、正离子模式、多反应监测方式,外标法定量,采用信息依赖采集扫描功能（IDA）结合增强子离子扫描（EPI）模式对检出阳性结果进行定性分析。结果方法的线性范围为1.0～200μg/L,8种青霉素及相应青霉噻唑酸在各种乳制品基质中均有良好的线性相关性,相关系数r在0.999 1～0.999 9之间,方法最低检测限为0.01～0.05μg/kg（固体乳粉）和0.002～0.010μg/kg（液体奶）;方法回收率在80.0%～110.0%,相对标准差为0.16%～7.06%。结论该方法测定8种青霉素药物及相应代谢产物青霉噻唑酸的残留量简便、快速、定性准确,可以满足对青霉素类药物及其代谢产物残留的检测要求。
Objective A ultra performance liquid chromatography-hybrid triple quadrupole linear ion-mass spectrometric method（UPLC-Qq QLIT）was established for determination of 8 penicilins（penicillin G,ampicillin,penicillin V,amoxicillin,nafcillin,cloxacillin,oxacillin and dicloxacillin）and their penicilloic acids（penicilloic acid G,ampicilloic acid,penicilloic acid V,amoxicilloic acid,nafcilloic acid,cloxacilloic acid,oxacilloic acid and dicloxacillioic acid）in milk products.The 8 penicilins and there penicilloic acids in milk products were surveyed.Methods The 8 penicilins and penicilloic acids in milk products were extracted by water in super-sonic instrument,proteins were precipitated by acetonitrile and degreased fat by n-hexane with liquid-liquid extraction,then the purified solution was concentrated by nitrogen,dissolved with acetonitrile-water（10 ∶ 90,V/V）and cleaned by 0.22 μm millipore filter.The filtrate was detected by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）,identified by electrospray ionization（ESI）in positive mode using multiple reaction monitoring,and quantified with external standards.Information dependent acquisition scan function（IDA）combined with enhanced production scan（EPI）was used to confirm the 8 penicilins and their penicilloic acids.Results The calibration curves of 8 penicilins and penicilloic acids showed good linearity in the range of 1.0-200 μg/L with correlation coefficients of 0.999 1-0.999 9.The detection limits of the method were 0.01-0.05 μg/kg for milk powder and 0.002-0.010 μg/kg for liquid milk.The recoveries of three spikinglevels ranged from 80.0% to 110.0%,and the relative standard deviations（RSD）were 0.16%-7.06%.Conclusion The method for determination of 8 penicilins and penicilloic acids in milk products by UPLC-Qq QLIT was of operation convenience,less interference from impurities and good accuracy,which could meet the requirements for the determination of 8 penicilins and penicilloic acids residues in milk products.
出处
《中国食品卫生杂志》
2016年第2期192-199,共8页
Chinese Journal of Food Hygiene
基金
深圳市科技创新委员会资助项目(JCYJ2013041102452855)
关键词
青霉素类药物
青霉噻唑酸
四极杆-串联线性离子阱质谱
乳制品
兽药残留
Penicillin
penicilloic acids
hybrid triple quadrupole linear ion trap-mass spectrometry
milk products
residue of veterinary drug
