摘要
建立水果中38种农药残留量的测定方法。样品经粉碎后,用1%甲酸-乙腈溶液快速提取,无水硫酸镁除水后,经C18、N-丙基乙二胺和硅藻土填料净化,用高效液相色谱-串联质谱仪分析。采用Accucore aQ柱进行分离,电喷雾正离子多反应监测模式检测,外标法定量。经方法验证,38种农药的方法检出限在0.3~26.2μg/kg之间,定量限在0.6~52.4μg/kg之间,线性相关系数(R)在0.9995~0.9999之间;本方法选择3个浓度水平进行添加回收实验(n=6),平均加标回收率在70.1%~119.3%之间,相对标准偏差在2.7%~12.4%之间。该方法前处理快速、灵敏、准确,可为水果中农药的监管提供技术支持。
A method for the determination of the residues of 38 pesticides in fruits was established.After being ground,the pesticide residues in samples were extracted with 1%acetic acid-acetonitril and dehydrated with anhydrous magnesium sulfate.Then,the pesticide residues in the supernatant were cleaned up with octadecylsilane(C18),primary secondary amine(PSA)and diatomite before being subjected to high performance liquid chromatography-tandem mass spectrometry(HPLCMS/MS)analysis.The separation was performed on an Accucore aQ column.The electrospray ionization mass spectrometry was operated in the positive mode using multiple reaction monitoring(MRM)and the analytes were quantified by the external standard method.The results indicated that the limits of detection(LODs)for all the pesticides were in the range of 0.3–26.2μg/kg,and the limits of quantitation(LOQs)ranged from 0.6 to 52.4μg/kg.The correlation coefficients(R)of the calibration curves were in the range of 0.9995–0.9999.The average recoveries at three spiked levels ranged from 70.1%to 119.3%(n=6)with relative standard deviations(RSDs)of 2.7%–12.4%.The method was rapid,sensitive and precise,and could provide technical support for the determination of pesticide residues in fruits.
作者
梁秀美
张维一
张微
谢拾冰
何如意
徐静
苏来金
孙博伦
张井
LIANG Xiumei;ZHANG Weiyi;ZHANG Wei;XIE Shibing;HE Ruyi;XU Jing;SU Laijin;SUN Bolun;ZHANG Jing(Experimental Station of Agricultural Products Quality Safety Risk Assessment,Ministry of Agriculture and Rural Affairs,Wenzhou Research Center of Characteristic Food Resources Engineering and Technology,Wenzhou Academy of Agricultural Sciences,Wenzhou 325006,China;Zhoushan Institute for Food and Drug Control,Zhoushan 316000,China;College of Food and Pharmaceutical Sciences,Ningbo University,Ningbo 315000,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2020年第8期288-296,共9页
Food Science
基金
浙江省科技厅公益性项目(2017C37087)。