CAJ | 학술논문

目的：建立同时测定乳制品中10种青霉素类抗生素残留的超高效液相色谱-串联质谱分析方法。方法样品经乙腈提取后,乙腈饱和正己烷除去脂肪,经0.22μm 微孔滤膜过滤,用乙腈-水(含0.1%甲酸5 mmol/L乙酸铵)为流动相, C18柱分离,20 min内梯度洗脱分离10种青霉素；电喷雾正离子模式电离(ESI+),多反应监测模式检测(MRM),外标法定量。结果在0.1~20μg/L浓度范围内,10种青霉素类药物在各种乳制品基质中均有良好的线性关系,线性相关系数均＞0.999；液体乳最低检测限为0.2μg/kg~1.0μg/kg,乳粉的最低检测限1.0μg/kg~5.0μg/kg；方法回收率在70.2%~108.2%,相对标准差为＜15%。结论该方法测定乳制品中10种青霉素药物的残留量简便、快速、准确,可以满足对青霉素类抗生素的监测要求。
목적：건립동시측정유제품중10충청매소류항생소잔류적초고효액상색보-천련질보분석방법。방법양품경을정제취후,을정포화정기완제거지방,경0.22μm 미공려막과려,용을정-수(함0.1%갑산5 mmol/L을산안)위류동상, C18주분리,20 min내제도세탈분리10충청매소；전분무정리자모식전리(ESI+),다반응감측모식검측(MRM),외표법정량。결과재0.1~20μg/L농도범위내,10충청매소류약물재각충유제품기질중균유량호적선성관계,선성상관계수균＞0.999；액체유최저검측한위0.2μg/kg~1.0μg/kg,유분적최저검측한1.0μg/kg~5.0μg/kg；방법회수솔재70.2%~108.2%,상대표준차위＜15%。결론해방법측정유제품중10충청매소약물적잔류량간편、쾌속、준학,가이만족대청매소류항생소적감측요구。
ABSTRACT:Objective To establish a method for simultaneous determination of 10 residual penicillin in dairy products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with acetonitrile and degreased with saturated acetonitrile n-hexane and filtered through 0.22μm millipore membrane. The filtrate was detected by ultra high performance liquid chromatography-tandem mass spectrometry, identified by electrospray ionization (ESI) in positive mode using multiple reactions monitoring mode, and quantified with external standard method. The sample extract was separated on a C18 column by gradient elution in 20 min with acetronitrile-water (containing 0.1% formic acid and 5 mmol/L ammonium acetate) as mobile phase.Results The calibration curve of the 10 penicillins residues showed a good linearity in the range of 0.1μg/L~20.0μg/L in various dairy products in the matrix with the correlation coefficientr2>0.999. The detection limit of the method was 0.2μg/kg~1.0μg/kg for liquid milk and 1.0μg/kg~5.0μg/kg for milk powder. The recoveries of spiking levels ranged from 70.2% to 108.2%, and the relative standard deviation (RSD) was less than 15%. ConclusionThe method for determination of residues of 10 penicillin antibiotics in dairy products is simple, rapid and accurate, and could satisfy the requirements for monitoring of penicillin residues <br> requirements for monitoring of penicillin residues