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Rapid Determination of Dipyrone Metabolite Residues in Foods of Animal Origin by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with a Through-type Solid phase Extraction |
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DOI: |
KeyWord:dipyrone metabolite through type solid phase extraction PRiME HLB ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS /MS) foods of animal origin |
Author | Institution |
ZHANG Jing-wen,ZHANG Hai-chao,FAN Bin,AI Lian-feng,WANG Jing,LI Wei,KANG Wei-jun |
1.Shijiazhuang Customs Technology Center;2.Hebei Food Inspection and Research Institute;3.School of Public Health,Hebei Medical University |
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Abstract: |
A method was developed for the rapid detection of 4-methylaminoantipyrine(MAA),4-aminoantipyrine(AA),4-formylaminoantipyrine(FAA) and 4-acetylaminoantipyrine(AAA) in foods of animal origin by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with a through type solid phase extraction.Samples were extracted with acetonitrile,then cleaned up with a PRiME HLB column,finally quantified by UPLC-MS/MS in MRM mode after gradient elution on an ACQUITY BEH C18 column with acetonitrile and 0.1% formic acid as mobile phases.Results showed that the calibration curves for four analytes were linear in the range of 0.5-50 μg/L with correlation coefficients(r) larger than 0.996.The limits of detection(LODs) and the limits of quantitation(LOQs) were 2 μg/kg and 5 μg/kg,respectively.The average recoveries at three spiked levels of 5,10 and 50 μg/kg ranged from 75.1% to 115%,with relative standard deviations(RSD) of 1.6%-7.4%.The proposed method is simple,rapid and accurate,and could be applied in the simultaneous determination of dipyrone metabolite residues in foods of animal origin. |
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