牛和猪肌肉组织中安乃近代谢物残留的液相色谱-串联质谱分析

Analysis of Dipyrone Metabolite Residues in Bovine Muscle and Porcine Muscle by Liquid Chromatography Coupled with Tandem Mass Spectrometry Detection

建立了牛和猪肌肉组织中安乃近代谢残留物4-甲酰氨基安替比林、4-乙酰氨基安替比林、4-氨基安替比林和4-甲基氨基安替比林的高效液相色谱-串连质谱（LC-M／MS）测定法。肌肉组织样品均质后，采用硫酸钠提取液提取。过滤后，过C18固相萃取（SPE）柱净化，采用LC-MS／MS电喷雾电离（ESI），多反应监测（MRM）模式检测。4-甲酰氨基安替比林和4-乙酰氨基安替比林采用外标法定量，而4-甲基氨基安替比林和4-氨基安替比林则是以4-异丙基氨基安替比林作为内标物采用内标法进行定量；4-甲酰氨基安替比林和4-氨基安替比林的检出限为1．0μ∥L；4-乙酰氨基安替比林和4-甲基氨基安替比林的检出限则为0．5μg／L；在添加浓度为5～200ng／g范围内，4-甲酰氨基安替比林的同收率为81．6％～94．0％；4-乙酰氨基安替比林的回收率为81．2％～90．2％；4-氨基安替比林的同收率为82％～101％；4-甲基氨基安替比林的回收率为78．5％～87．0％；相对标准偏差（RSD）均在7％以内。

A method had been developed for the determination of dipyrone metabolite residues, 4-formylaminoantipyrine （ FAA ）, 4-acetylaminoantipyrine （ AAA ）, 4-aminoantipyrine （ AA ） and 4-methylaminoantipyrine （MAA） in bovine and pork muscle. Homogenized muscle samples were extracted with Na2SO4 sdlution. After filtration, the extracts were then cleaned by C18 solid phase extraction （SPE） cartridge. Identification was achieved by electrospray ionization （ESI） in positive mode using multiple reaction monitoring. FAA and AAA were quantified by external standard method, while AA and MAA were measured by internal standard methold using isopropylaminoantipyrine as internals standard. Limits of detection of FAA and AA were 1.0 μg/L, while those of AAA and MAA were 0.5 μg/L. The recoveries of FAA, AAA, AA and MAA were 81.6% - 94.0%, 81. 2% -90.2%, 82% - 101% and 75. 0% -86.4%, respectively at the spiked levels of 5 -20 ng/g. The RSD of the method was less than 7%.