液相色谱-串联质谱法测定河豚鱼和鳗鱼中 9种青霉素类抗生素
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1.0~20 μg/kg(LOQ~10LOQ)范围时, 方法线性关系良好, 相关系数大于0.999。在LOQ、2 LOQ、4 LOQ、10 LOQ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1.0 μg/kg; 阿莫西林、氨苄西林、氯唑西林、双氯西林为2.0 μg/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 A sensitive method was developed for the determination of 9 penicillins in Fugu and eel by high pressure liquid chromatography-electrospray tandem mass spectrometry (HPLC-MS/MS). Methods Samples were extracted with acetonitrile-ammonia water, separated on a C18 column by gradient elution with acetonitrile and 0.3% acetic acid solution as mobile phase. Identification was achieved by electrospray ionization(ESI) in positive mode. Results The method showed a good linearity over the range of 1.0~20 μg/kg for 9 compounds of penicillins with r≥0.999. Recoveries of 9 penicillins were between 81.4% and 109.7% (n=6) at spiked levels of LOQ, 2LOQ, 4LOQ and 10LOQ with relative standard deviations (RSD of 2.81%?7.12%). The limit of quantitation(LOQ) for nafcillin, penicillin G, piperacillin, penicillin V and ox-acillin were 1.0 μg/kg and the LOQ for amoxicillin, ampicillin, cloxacillin and dicloxacillin were 2.0 μg/kg. Conclusion This method is sensitive and accurate, and it is suitable for the analysis of 9 penicillins in aquatic products.
标题：液相色谱-串联质谱法测定河豚鱼和鳗鱼中 9种青霉素类抗生素
英文标题：Determination of 9 penicillins in Fugu and eel by high pressure liquid chromatography-electrospray tandem mass spectrometry
作者：
李学民 秦皇岛出入境检验检疫局
曹彦忠 秦皇岛出入境检验检疫局
张进杰 秦皇岛出入境检验检疫局
母健 秦皇岛出入境检验检疫局
王蕾 秦皇岛出入境检验检疫局
王贺琴 秦皇岛出入境检验检疫局
中文关键词:液相色谱-串联质谱法,青霉素,河豚鱼,鳗鱼,
英文关键词:high pressure liquid chromatography-electrospray tandem mass spectrometry (HPLC-MS-MS),penicillins,Fugu,eel,
发表日期：2013-06-15
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