利用液相層析串聯質譜儀檢測豬肝中動物用藥殘留之多重分析法

Simultaneous Determination of Multiclass Veterinary Drug Residues in Porcine Liver by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

盧信芳(Hsin-Fang Lu) ； 唐玉芸(Yu-Yun Tang) ； 林旭陽(Hsu-Yang Lin) ； 黃登福(Deng-Fwu Hwang) ； 闕麗卿(Lih-Ching Chiueh) ； 羅吉方(Chi-Fang Lo)

《臺灣農業化學與食品科學》 49卷2期 (2011/04) Pp. 64-73

https://doi.org/10.6578/TJACFS.2011.009

摘要

本試驗方法使用液相層析串聯質譜儀(liquid chromatography/tandem mass spectrometry, LC/MS/MS)，以電灑游離正離子法，進行豬肝中巨環類(macrolides)抗生素、β-內醯胺類(β-lactam)抗生素、林可黴素類(lincosamides)抗生素及其他類抗生素之方法開發。研究中針對檢測豬肝中殘留15種抗生素之快速多重殘留分析方法進行開發。試驗步驟為肝臟檢體以甲醇、Na2EDTA水溶液及乙腈萃取，以矽藻土淨化之萃取液，經氮氣濃縮後，選用Acquity UPLC HSS T3之層析管柱，搭配0.005%甲酸水溶液與乙腈進行分析。此方法之平均回收率大多介於50.2~115.8%間，平均變異係數為2.8~15.1%，檢測限量介於0.25~10 ppb。本研究提供了一個快速且敏感的多重殘留分析方法，可同時檢測豬肝中15種品項之動物用藥。

關鍵字

液相層析串聯質譜法 ； 巨環類 ； β-內醯胺類 ； 林可黴素類

並列摘要

We described a method by using liquid chromatography tandem mass spectrometry (LC/MS/MS) combined with positive electrospray ionization to identify different classes of antibiotics (macrolides, β-lactam antibiotics, lincosamides and miscellaneous antibiotics). The aim of this study was to develop a rapid method for simultaneous determination of 15 antibiotics in porcine liver. Sample preparation was performed using liquid/liquid extraction with methanol, Na2EDTA and acetonitrile. The extracts were cleaned up with Hyflo Supercel and were evaporated to dryness under a stream of nitrogen. The chromatography was carried out on a Acquity UPLC HSS T3 column as mobile phase component A was water with 0.005% formic acid, and component B was acetonitrile. The average recoveries were 50.2% to 115.8%, and coefficients of variation were from 2.8% to 15.1%, indicating this method is reliable. Estimated limits of quantification were 0.25-10 ppb. In this paper, a rapid and sensitive multiclass method had been developed on simultaneous determination of 15 antibiotics in porcine liver.

並列關鍵字

Liquid Chromatography Tandem Mass Spectrometry ； LC/MS/MS ； macrolides ； β-lactam ； lincosamides