CAJ | 학술논문

建立了快速测定牛奶中季铵类化合物多残留的固相萃取-高效液相色谱-串联质谱法。以乙腈提取目标化合物,弱阳离子固相萃取柱萃取净化,氮吹浓缩处理,C18色谱柱分离,0.1%乙酸-20 mmol/L乙酸铵甲醇溶液梯度洗脱,多反应监测正离子模式扫描。目标化合物在7 min内实现良好分离,并在各自相应浓度范围内线性良好,相关系数>0.99,方法的定量限：十二烷基二甲基苄基溴化铵、十四烷基三甲基溴化铵、十四烷基二甲基苄基氯化铵和双十烷基二甲基溴化铵为0.2μg/kg；十六烷基三甲基溴化铵为1.0μg/kg。在2.0,10和20μg/kg添加浓度,目标化合物在纯牛奶、鲜牛奶和低脂牛奶中的平均回收率分别为70.5%~96.6%,69.1%~87.9%和67.1%~93.3%,相对标准偏差为1.4%~11.6%。本方法操作简便,灵敏度高,适用于牛奶中季铵类化合物多残留的快速检测。
건립료쾌속측정우내중계안류화합물다잔류적고상췌취-고효액상색보-천련질보법。이을정제취목표화합물,약양리자고상췌취주췌취정화,담취농축처리,C18색보주분리,0.1%을산-20 mmol/L을산안갑순용액제도세탈,다반응감측정리자모식소묘。목표화합물재7 min내실현량호분리,병재각자상응농도범위내선성량호,상관계수>0.99,방법적정량한：십이완기이갑기변기추화안、십사완기삼갑기추화안、십사완기이갑기변기록화안화쌍십완기이갑기추화안위0.2μg/kg；십륙완기삼갑기추화안위1.0μg/kg。재2.0,10화20μg/kg첨가농도,목표화합물재순우내、선우내화저지우내중적평균회수솔분별위70.5%~96.6%,69.1%~87.9%화67.1%~93.3%,상대표준편차위1.4%~11.6%。본방법조작간편,령민도고,괄용우우내중계안류화합물다잔류적쾌속검측。
A method was proposed for the determination of the residues of the quaternary ammonium compounds ( QACs) in milk by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS ) . The sample was extracted with acetonitrile, cleaned-up by weak cationic exchange solid phase extraction cartridge and concentrated in a gentle nitrogen stream. The separation of 5 QACs was performed on a Thermo C18 column (150 mmí2. 1 mm, 3 μm) using gradient elution of 0. 1%acetic acid and 20 mmol/L ammonium acetate methanol as the mobile phase within 7 min. The QACs were analyzed under the multiple reaction monitoring ( MRM ) mode with positive electrospray ionization. The calibration curves were linear well with correlation coefficient over 0 . 99 . The limit of quantification of the method was 1 . 0 μg/kg for hexadecyltrimethyl ammonium bromide and 0 . 2 μg/kg for benzyldodecyldimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide, benzyldimethyltetradecyl ammonium chloride and didecyldimethyl ammonium bromide. The average recoveries for 5 QACs were between 70. 5% and 96. 6% in pure milk, between 69. 1% and 87. 9% in fresh milk and between 67. 1% and 93. 3% in low fat milk at the spiked levels of 2, 10 and 20 μg/kg, with relative standard derivation ( RSD) from 1. 4% to 11. 6%. The developed method is simple and sensitive, and suitable for rapid analysis of quaternary ammonium compounds in the milk.