QuEChERS-超高效液相色谱串联质谱法测定大米中30种农药残留
QuEChERS-Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of 30 Pesticide Residues in Rice
李丹娜 1王建山2
作者信息
- 1. 河南应用技术职业学院,郑州 450042
- 2. 陕西省食品药品检验研究院,西安 710065;陕西省食品药品安全监测重点实验室,西安 710065
- 折叠
摘要
采用QuEChERS前处理技术,结合超高效液相色谱串联质谱联用仪,建立大米中30种农药残留的测定方法.优化样品的提取溶剂、净化方式、液相色谱的分离条件和质谱参数等技术指标,采用优化后的条件,大米样品经体积分数1％乙酸乙腈提取,QuEChERS法净化后,用体积分数0.1％甲酸水(含2 mmol/L甲酸铵)和甲醇为流动相,经Eclipse Plus C18(2.1 mm ×50.0 mm,1.8 μm)分离,采用电喷雾电离(ESI)和多离子检测模式(MRM)进行检测,基质外标法定量.30种农药的质量浓度在0.001～0.050 mg/L内与峰响应呈线性关系,线性相关系数均大于0.995,定量限(10S/N)在0.02～2.98 μg/kg,在3～30 μg/kg添加浓度范围内,平均回收率在70.3％～109.8％,相对标准偏差在1.1％～11.4％.
Abstract
The determination method of 30 pesticide residues in rice was established by use of QuEChERS prepa-ration technique and combination of ultra-high-performance liquid chromatography-tandem mass spectrometry.The technical indexes,including extraction solvent,purification method,chromatographic separation conditions and mass spectrometry parameters,etc.were optimized.Under the optimized conditions,rice samples were extracted by 1％acetic acid acetonitrile,purified by QuEChERS method,and with 0.1％formic acid water(containing 2 mmol/L ammonium formate)and methanol as mobile phases.Chromatographic separation was achieved by use of Eclipse Plus C18(2.1 mm ×50.0 mm,1.8 μm).Detection was performed by use of electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode,and matrix-matched calibration was used for quantification.The calibration curves of the 30 pesticides indicated good linearity over the concentration range of 0.001-0.050 mg/L,with correlation coefficients greater than 0.995.The limits of quantification(LOQs)were between 1 μg/kg and 10μg/kg,and the recoveries ranged from 70.3％to 109.8％with relative standard deviations(n=6)of 1.1％～11.4％in the range of 3-30 μg/kg.
关键词
QuEChERS/UPLC-MS/MS/大米/农药残留Key words
QuEChERS/UPLC-MS/MS/rice/pesticide residue引用本文复制引用
基金项目
2019年陕西省创新能力支撑计划项目(2019PT-22)
出版年
2024
NETL
NSTL
万方数据