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Determination of marker residue of Olaquindox in fish tissue by ultra performance liquid chromatography–tandem mass spectrometry
Author(s) -
Zhang Xiaojun,
Zheng Bin,
Zhang Hong,
Chen Xuechang,
Mei Guangming
Publication year - 2011
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201000722
Subject(s) - chromatography , chemistry , tandem mass spectrometry , mass spectrometry , residue (chemistry) , liquid chromatography–mass spectrometry , fish <actinopterygii> , tandem , high performance liquid chromatography , biology , materials science , biochemistry , fishery , composite material
Methyl‐3‐quinoxaline‐2‐carboxylic acid (MQCA) is the last major remaining detectable metabolite of Olaquindox in animal tissue. A rapid, sensitive and specific ultra performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for the detection and quantification of MQCA in fish tissue using deuterated quinoxaline‐2‐carboxylic acid (d 4 ‐QCA) as internal standard. Various parameters affecting sample preparation, LC separation and MS/MS detection were investigated, and the optimal conditions concerned were determined. Fish tissue samples were subject to hydrochloric acid hydrolysis followed by Oasis MAX solid‐phase extraction clean‐up; analysis was performed using UPLC coupled to electrospray MS/MS. The chromatographic separation was achieved in less than 5 min. The limit of detection and the limit of quantification were 0.1 and 0.25 ng/g, respectively. The average recoveries of MQCA, spiked at levels of 0.25–50.0 ng/g, were from 92.7 to 104.3%. The relative standard deviation values were <6%. The validated method was successfully applied to analyze 60 batch samples collected from the local market.