CAJ | 학술논문

建立了牛奶和奶粉中卡巴氧代谢物喹喔啉-2-羧酸(QCA)和喹乙醇代谢物3-甲基喹喔啉-2-羧酸(MQCA)残留量的液相色谱-串联质谱测定方法. 将样品经0.6% (体积分数)的甲酸溶液进行消化, 用Tris缓冲溶液调节pH后, 加入Protease蛋白酶进行酶解, 样品溶液用0.3 mol/L HCl溶液酸化后, 采用阴离子交换固相萃取柱Oasis MAX进行净化和富集. 分析样品以0.1% (体积分数)的甲酸溶液-甲醇-乙腈为流动相, 经Inertsil ODS-3色谱柱分离, 采用负离子扫描, 在LC-MS/MS多反应监测模式下进行定性及定量分析. 喹口恶啉-2-羧酸和3-甲基喹口恶啉-2-羧酸的方法测定下限牛奶为0.5 μg/kg, 奶粉为4.0 μg/kg. 对牛奶在0.5～5.0 μg/kg, 奶粉在4.0～40.0 μg/kg添加水平的平均回收率为68.2%～82.5%, RSD为3.4%～12%.
건립료우내화내분중잡파양대사물규악람-2-최산(QCA)화규을순대사물3-갑기규악람-2-최산(MQCA)잔류량적액상색보-천련질보측정방법. 장양품경0.6% (체적분수)적갑산용액진행소화, 용Tris완충용액조절pH후, 가입Protease단백매진행매해, 양품용액용0.3 mol/L HCl용액산화후, 채용음리자교환고상췌취주Oasis MAX진행정화화부집. 분석양품이0.1% (체적분수)적갑산용액-갑순-을정위류동상, 경Inertsil ODS-3색보주분리, 채용부리자소묘, 재LC-MS/MS다반응감측모식하진행정성급정량분석. 규구악람-2-최산화3-갑기규구 악람-2-최산적방법측정하한우내위0.5 μg/kg, 내분위4.0 μg/kg. 대우내재0.5～5.0 μg/kg, 내분재4.0～40.0 μg/kg첨가수평적평균회수솔위68.2%～82.5%, RSD위3.4%～12%.
This study presented a liquid chromatography-tandam mass spectrometry (LC-MS/MS) method for determination of residues of Carbadox, Olaquindox and related metabolites quinoxalie-2-carboxylic acid(QCA) and 3-methylquinoxaline-2-carboxylic acid (MQCA) in milk and milk powder. As for the extraction of QCA and MQCA, milk and milk powder is first digested with 0.6% formic acid to deactivate naturally-occurring enzymes. After overnight enzymatic hydrolysis with protease, the tissue extract is acidified, centrifuged and filtered. QCA and MQCA are recovered from the tissue extract by using an Oasis MAX solid phase extraction (SPE) cartridge. The analytes are separated on a Inertsil ODS-3 LC column, and qualitatively and quantitatively determined under multi-reaction monitoring (MRM) scan type with tandem mass analyzer using positive polarity mode. The limit of quatitation (LOQ) for the two analytes in milk is 0.5 μg/kg, in milk power is 4.0 μg/kg. At the spiked level in the range of 0.5～5.0 μg/kg in milk and 4.0～40.0 μg/kg in milk power, the mean recoveries are in the range of 68.2%～82.5%, the relative standard deviation are in the range of 3.4%～12%.