首页|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

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

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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.
Determination of 47 pesticide resides in sucrose by UPLC-MS/MS
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.

sucrosepesticide residuesliquid chromatography-mass spectrometrymulti reaction monitoring mode(MRM)matrix effectinternal standard method

谭菊英、蒋洁、刘庄蔚、何虹、杨欣智、朱健萍、邓鸣、徐光辉、王健、赵庄、卢日刚

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广西壮族自治区药品检验研究院,南宁 530021

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

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

广西重点研发计划项目广西科技重大专项计划项目

桂科AB22035032桂科AA22117005

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(6)