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目的建立高压液相色谱-电喷雾串联质谱(HPLC-MS-MS)同时测定河豚鱼和鳗鱼中9种青霉素残留量的检测方法。方法样品经乙腈-氨水溶液提取后,用C18色谱柱分离,乙腈-乙酸为流动相梯度洗脱,最后采用液相色谱-电喷雾串联质谱在正离子多反应监测模式下测定。结果在1.0～20μg/kg(LOQ～10LOQ)范围时,方法线性关系良好,相关系数大于0.999。在LOQ、2LOQ、4LOQ、10LOQ四个添加水平下青霉素的回收率在81.4%～109.7%之间,相对标准偏差在2.81%～7.12%之间,方法检出限是:萘夫西林、青霉素G、哌拉西林、青霉素V、苯唑西林为1.0μg/kg;阿莫西林、氨苄西林、氯唑西林、双氯西林为2.0μg/kg。结论此方法灵敏度高,准确性好,适用于水产品中青霉素的定量检测。
OBJECTIVE To establish a method for simultaneous determination of 9 penicillin residues in puffer fish and eel by high pressure liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-MS-MS). Methods The sample was extracted with acetonitrile-ammonia solution, separated on a C18 column and eluted with acetonitrile-acetic acid as the mobile phase. The liquid chromatography-electrospray ionization tandem mass spectrometry (ESI-MS / MS / MS) Results The linearity was good with the range of 1.0 ~ 20μg / kg (LOQ ~ 10LOQ), and the correlation coefficient was greater than 0.999. The recoveries of penicillin at LOQ, 2LOQ, 4LOQ and 10LOQ were between 81.4% and 109.7% with relative standard deviations between 2.81% and 7.12%. The detection limits were as follows: nafcillin, penicillin G , Piperacillin, penicillin V, oxacillin 1.0μg / kg; amoxicillin, ampicillin, cloxacillin, dicloxacillin 2.0μg / kg. Conclusion This method has high sensitivity and good accuracy and is suitable for the quantitative detection of penicillin in aquatic products.