超高效液相色谱-串联质谱检测蔗糖中47种农药残留量的方法
Determination of 47 pesticide resides in sucrose by UPLC-MS/MS
谭菊英 1蒋洁 1刘庄蔚 1何虹 1杨欣智 1朱健萍 1邓鸣 1徐光辉 2王健 3赵庄 1卢日刚1
作者信息
- 1. 广西壮族自治区药品检验研究院,南宁 530021
- 2. 中粮崇左糖业有限公司/广西壮族自治区甘蔗产业链延伸工程研究中心,崇左 532200
- 3. 中粮崇左糖业有限公司/广西壮族自治区甘蔗产业链延伸工程研究中心,崇左 532200;中粮营养健康研究院有限公司/营养健康与食品安全北京市重点实验室,北京 102209
- 折叠
摘要
目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定蔗糖中47种农药残留量的方法.方法:蔗糖样品经酸性乙腈提取,氮气吹干浓缩,采用LC-MS/MS进行分析检测,在多反应检测模式(MRM)下,用空白基质标准曲线-内标法进行定量.结果:各待测物质在一定浓度范围内线性良好(r＞0.995),检测限为0.01～2.00 μg·kg-1.分别在蔗糖样品中添加47种农药标准溶液10、25、50 μg·kg-1,进行标准添加回收试验,方法回收率为71.0％～106.0％,重复性RSD为0.90％～8.5％.15批蔗糖样品中2批检出噻虫嗪、噻虫胺,其余均未检出.结论:该方法具有前处理简单快捷、灵敏、准确等优点,符合农药残留检测要求,满足蔗糖中农药残留检测需要,可用于蔗糖的质量控制.
Abstract
Objective:To establish a UPLC-MS/MS method for the simultaneous determination of 47 pesticide residues in Sucrose.Methods:The residues in the sample were extracted by acidic acetonitrile,concentrated by blow dry with nitrogen gas and then analyzed by using LC-MS/MS with multiple reaction monitoring(MRM).Blank matrix standard curve with internal standard method was used to determine the residue contents.Results:Each substance to be tested had good linearity relationship within certain concentration(r＞0.995).The limits of quantification(LOQ)were 0.01-2.00 μg·kg-1.The recoveries of 47 pesticide residues at three levels of 10,25 and 50 µg·kg-1 were from 71.0％to 106.0％with the RSD of 0.90％-8.5％in sucrose.2 batches in 15 batches of sucrose samples were detected thiamethoxam and thiamethoxam,while the rest were not detected.Conclusion:The method is simple,rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the determination of analysis,and this developed procedure is suitable for the determina-tion of pesticide residues in Sucrose,can be used for quality control of sucrose.
关键词
蔗糖/农药残留/液相色谱-质谱/多反应监测模式/基质效应/内标法Key words
sucrose/pesticide residues/liquid chromatography-mass spectrometry/multi reaction monitoring mode(MRM)/matrix effect/internal standard method引用本文复制引用
基金项目
广西重点研发计划项目(桂科AB22035032)
广西科技重大专项计划项目(桂科AA22117005)
出版年
2024
NETL
NSTL
万方数据