CAJ | 학술논문

建立了牛奶中4种安乃近代谢物--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液相色谱-串连质谱(LC-M/MS)测定法.样品加入TRIS缓冲溶液后用乙腈提取,提取液经乙腈饱和过的正己烷脱脂净化,采用LC-MS/MS电喷雾正离子(ESI+)、多反应监测(MRM)模式榆测,4-乙酰氨基安替比林、4-甲酰氨基安替比林和4-氨基安替比林采用外标法定量,4-甲基氨基安替比林采用内标法进行定量.4-甲酰氨基安替比林的检出限为0.24 μg/kg,4-氨基安替比林的检出限为0.59 μg/kg,4-乙酰氨基安替比林的检出限为0.20 μg/kg,4-甲基氨基安替比林的检出限则为0.61 μg/kg.在添加量5～20 μg/kg范围内,4种安乃近的回收率在80.4%～97.9%范围内,相对标准偏差(RSD)均小于9%.
건립료우내중4충안내근대사물--4-갑선안기안체비림、4-을선안기안체비림、4-안기안체비림화4-갑기안기안체비림적액상색보-천련질보(LC-M/MS)측정법.양품가입TRIS완충용액후용을정제취,제취액경을정포화과적정기완탈지정화,채용LC-MS/MS전분무정리자(ESI+)、다반응감측(MRM)모식유측,4-을선안기안체비림、4-갑선안기안체비림화4-안기안체비림채용외표법정량,4-갑기안기안체비림채용내표법진행정량.4-갑선안기안체비림적검출한위0.24 μg/kg,4-안기안체비림적검출한위0.59 μg/kg,4-을선안기안체비림적검출한위0.20 μg/kg,4-갑기안기안체비림적검출한칙위0.61 μg/kg.재첨가량5～20 μg/kg범위내,4충안내근적회수솔재80.4%～97.9%범위내,상대표준편차(RSD)균소우9%.
A liquid chromatography coupled with tandem mass spectrometric(LC-MS/MS)method was proposed for the determination of four dipyrone metabolites in milk,i.e.,4-methylaminoantipyrine(MAA),4-formylaminoantipyrine(FAA),4aminoantipyrine(AA),4-acetylaminoantipyrine(AAA).Samples were extracted with acetonitrile,and the resulting extract was then cleaned up/defatted with acetonitrile-saturated n-hexane and concentrated by rotary evaporation prior to LC-MS/MS with positive electrospray ionization(ESI)in the multiple reaction monitoring(MRM)mode.FAA,AAA and AA were quantified by the external standard method,while MAA by the internal standard method.The limits of detection of FAA,AAA,AA and MAA by the method were 0.24,0.20,0.59 μg/kg and 0.61 μg/kg,respectively.Mean recoveries in blank samples at three spike levels (5,10,20 μp/kg)ranged between 80.4% and 97.9%,with relative standard deviations less than 9%(n = 10).