CAJ | 학술논문

　　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、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。
　　목적건립고압액상색보-전분무천련질보(HPLC-MS-MS)동시측정하돈어화만어중9충청매소잔류량적검측방법。방법양품경을정-안수용액제취후，용C18색보주분리，을정-을산위류동상제도세탈，최후채용액상색보-전분무천련질보재정리자다반응감측모식하측정。결과재1.0~20μg/kg(LOQ~10LOQ)범위시，방법선성관계량호，상관계수대우0.999。재LOQ、2 LOQ、4 LOQ、10 LOQ사개첨가수평하청매소적회수솔재81.4%~109.7%지간，상대표준편차재2.81%~7.12%지간，방법검출한시：내부서림、청매소 G、고랍서림、청매소 V、분서서림위1.0μg/kg；아막서림、안변서림、록서서림、쌍록서림위2.0μg/kg。결론차방법령민도고，준학성호，괄용우수산품중청매소적정량검측。
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 electro-spray ionization(ESI) in positive mode. Results The method showed a good linearity over the range of 1.0~20μg/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 oxacil-lin 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.