超高效液相色谱-串联质谱法测定桃中春雷霉素残留量  

Determination of Kasugamycin Residues in Peach by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘炜[1] 刘行[2] 杨晓凤[1] 尹全[1] 毛建霏[1] 张义蓉[1] 陈龙飞 LIU Wei;LIU Xing;YANG Xiaofeng;YIN Quan;MAO Jianfei;ZHANG Yirong;CHEN Longfei(Analysis and Testing Center,Sichuan Academy of Agricultural Sciences,Chengdu 610066,China;Institute of Economic Crops,Sichuan Academy of Agricultural Sciences,Chengdu 610300,China)

机构地区：[1]四川省农业科学院分析测试中心,四川成都610066 [2]四川省农业科学院经济作物育种栽培研究所,四川成都610300

出　　处：《山西农业科学》2020年第8期1224-1226,1320,共4页Journal of Shanxi Agricultural Sciences

基　　金：西藏自治区重点科技计划项目(XZ201801NB07)。

摘　　要：建立了利用超高效液相色谱-串联质谱测定桃中春雷霉素残留量的分析方法。样品经1.0%甲酸-甲醇提取,氯化钠盐析后,取1.0 mL提取液,经Waters ACQUITY UPLC BEH Amide Column分离,乙腈∶0.2%甲酸水为60∶40(V/V)作为流动相进行等度洗脱,经电喷雾离子源正离子化,多反应监测(MRM)模式检测,基质匹配标准曲线外标法定量。结果表明,春雷霉素在10~1000μg/kg的范围内线性关系良好,相关系数为0.999;10、100、200μg/kg等3个添加水平的平均添加回收率分别为86.2%、91.0%、89.5%,相对标准偏差RSD(n=7)分别为2.2%、3.7%、4.5%,方法检出限为3.0μg/kg,定量限为10.0μg/kg。该方法快速、简便、准确,可满足桃中春雷霉素的残留检测要求,为春雷霉素的科学使用以及在食品中的残留分析和风险评估提供重要依据。A method of determination of Kasugamycin in peach by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed.The peach was extracted with 1.0%formic acid-methanol,after salting out of anhydrous sodium chloride,1.0 mL extraction solvent were separated on a Waters ACQUITY UPLC BEH Amide Column with gradient elution of acetonitrile-0.2%formic acid water(V/V=60∶40)as mobile phases,and the qualitative and quantitative analyses were performed under positive electrospray ionization(ESI+)in multiple reaction monitoring(MRM)mode,with the matrix-matched calibrations.The result showed that satisfactory linearity in the concentration range of 10-1000μg/kg for Kasugamycin was obtained,and correlation coefficients was 0.999.Average recoveries of Kasugamycin added to peach ranged from 86.2%to 91.0%,with relative standard deviations(RSD)from 2.2%to 5.1%.The limits of detection was 3.0μg/kg,and the limits of quantification was 10.0μg/kg for Kasugamycin.The method is quick,easy,effective,accurate and can meet the requirements for the determination of Kasugamycin in peach,can provide an important basis for the scientific use of Kasugamycin and the residual analysis and risk assessment of Kasugamycin in food.

关 键 词：超高效液相色谱-串联质谱 春雷霉素 桃 残留量 

分 类 号：O657.63[理学—分析化学]