液质联用法测定饲料原料乳清粉中的喹烯酮含量
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摘要
建立了液质联用法测定饲料原料乳清粉中喹烯酮含量的方法。饲料原料乳清粉经20%乙腈溶液(含0.2%甲酸)超声提取,PRiME HLB固相萃取柱净化,0.22μm滤膜过滤,经液质联用仪基质加标外标法定量测定。试验结果表明,喹烯酮浓度在20～1 000 ng/ml范围内呈良好的线性关系(R~2=0.999 1)。向空白乳清蛋白粉中添加喹烯酮含量为20、50、100、500μg/kg时,回收率在79.9%～90.8%之间,定量限为10μg/kg。本检测方法具有较高的准确度、灵敏度、稳定性,可满足饲料原料乳清粉中喹烯酮的含量检测。
A new method for determination of quinolone in whey powder of feed by liquid chromatography-tendem mass spectrometry(LC-MS/MS) was established. Whey powder was extracted by 20% acetonitrile solution(0.2% formic acid), and cleaned by PRiME HLB solid phase extraction column, filtered by 0.22 μm filter membrane, and determined by LC-MS/MS matrix plus external standard method. Good linearity(R~2=0.999 1) was observed in the range 20～1 000 ng/ml. When the content of quinolone in whey powder was 20, 50, 100 and 500 μg/kg, the recoveries ranged between 79.9%～90.8%,and the limit of detection was 10 μg/kg. The method has high accuracy, sensitivity and stability, and can be used for the determination of quinolone in whey powder of feed.
A new method for determination of quinolone in whey powder of feed by liquid chromatography-tendem mass spectrometry(LC-MS/MS) was established. Whey powder was extracted by 20% acetonitrile solution(0.2% formic acid), and cleaned by PRiME HLB solid phase extraction column, filtered by 0.22 μm filter membrane, and determined by LC-MS/MS matrix plus external standard method. Good linearity(R~2=0.999 1) was observed in the range 20～1 000 ng/ml. When the content of quinolone in whey powder was 20, 50, 100 and 500 μg/kg, the recoveries ranged between 79.9%～90.8%,and the limit of detection was 10 μg/kg. The method has high accuracy, sensitivity and stability, and can be used for the determination of quinolone in whey powder of feed.
引文
[1]王继强,赵中生,李爱琴,等.乳清粉的营养特性及在乳仔猪饲料上的应用[J].饲料广角,2011(20):32-34.
[2]王茂兴.高低蛋白乳清粉对保育仔猪生产性能的对比试验[J].福建畜牧兽医,2015(37):7-8.
[3]周雪梅,杨在宾,于彩云,等,含脂乳清和浓缩蛋白乳清对断奶仔猪生长性能的影响研究[J].猪业科学,2017(34):90-93.
[4]詹黎明,郭吉余,吴德.乳清浓缩蛋白的免疫调节作用及其在仔猪生产中的应用[J].中国饲料,2012(18):10-12.
[5]曾英华,方热军.喹烯酮的研究及应用概况[J].湖南饲料,2010(6):90-93.
[6]李娟,刘东升,许东宝,等.喹烯酮对仔猪生产性能影响的研究[J].中国饲料,2005(23):27-28.
[7]陈倩.喹噁啉类药物致HepG2细胞氧化损伤及S期阻滞调控机理研究[D].北京:中国农业大学,2009.
[8]农业部2086号公告-5-2014饲料中卡巴氧、乙酰甲喹、喹烯酮和喹乙醇的测定液相色谱-串联质谱法[S].2014.
[9]刘元元,张丽芳,邹思湘,等.高效液相色谱法测定鱼饲料中的喹烯酮[J].畜牧与兽医,2007,39(1):35-37.
[10]贾涛.高效液相色谱法检测饲料中喹烯酮的探讨[J].饲料广角,2011(3):33-41.
[11]贾涛.液相色谱-二极管阵列法测定饲料中喹烯酮[J].饲料研究,2012(9):73-76.
[12]顾亮,徐彦辉,蒋俊树,等.高效液相色谱串联质谱法测定饲料中喹烯酮含量[J].化学分析计量,2010,19(5):52-54.
[13]刘发全,曾明华,许世富,等.同时测定饲料中乙酰甲喹、喹乙醇、喹烯酮3种药物方法的研究[J].现代农业科技,2008(24):230-232.
[2]王茂兴.高低蛋白乳清粉对保育仔猪生产性能的对比试验[J].福建畜牧兽医,2015(37):7-8.
[3]周雪梅,杨在宾,于彩云,等,含脂乳清和浓缩蛋白乳清对断奶仔猪生长性能的影响研究[J].猪业科学,2017(34):90-93.
[4]詹黎明,郭吉余,吴德.乳清浓缩蛋白的免疫调节作用及其在仔猪生产中的应用[J].中国饲料,2012(18):10-12.
[5]曾英华,方热军.喹烯酮的研究及应用概况[J].湖南饲料,2010(6):90-93.
[6]李娟,刘东升,许东宝,等.喹烯酮对仔猪生产性能影响的研究[J].中国饲料,2005(23):27-28.
[7]陈倩.喹噁啉类药物致HepG2细胞氧化损伤及S期阻滞调控机理研究[D].北京:中国农业大学,2009.
[8]农业部2086号公告-5-2014饲料中卡巴氧、乙酰甲喹、喹烯酮和喹乙醇的测定液相色谱-串联质谱法[S].2014.
[9]刘元元,张丽芳,邹思湘,等.高效液相色谱法测定鱼饲料中的喹烯酮[J].畜牧与兽医,2007,39(1):35-37.
[10]贾涛.高效液相色谱法检测饲料中喹烯酮的探讨[J].饲料广角,2011(3):33-41.
[11]贾涛.液相色谱-二极管阵列法测定饲料中喹烯酮[J].饲料研究,2012(9):73-76.
[12]顾亮,徐彦辉,蒋俊树,等.高效液相色谱串联质谱法测定饲料中喹烯酮含量[J].化学分析计量,2010,19(5):52-54.
[13]刘发全,曾明华,许世富,等.同时测定饲料中乙酰甲喹、喹乙醇、喹烯酮3种药物方法的研究[J].现代农业科技,2008(24):230-232.