QuEChERS-UPLC-MS/MS测定大米中氯虫苯甲酰胺和五氟磺草胺的残留
Determination of chlorantraniliprole and penoxsulam residues in rice by QuEChERS-UPLC-MS/MS
黄子杰 1黄朋勉 1罗宽能 2向忠平 2张洪刚2
作者信息
- 1. 怀化市疾病预防控制中心,湖南怀化 418000
- 2. 长沙理工大学化学化工学院,湖南长沙 410114
- 折叠
摘要
目的:建立一种新的QuEChERS-超高效液相色谱—串联质谱(UPLC-MS/MS)检测大米中氯虫苯甲酰胺和五氟磺草胺的残留方法.方法:样品经0.2％甲酸—乙腈提取后,N丙基乙二胺(PSA)和石墨化碳黑(GCB)填料净化,以0.2％甲酸水—乙腈为流动相梯度洗脱,经C18色谱柱分离,采用UPLC-MS/MS测定.结果:氯虫苯甲酰胺和五氟磺草胺的定量限(LOQ)均为0.004 mg/kg,方法检出限(LOD)均为0.001 mg/kg.两种待测农药在0.002～0.5 mg/L质量浓度范围内呈良好的线性关系,其相关系数均在0.993以上.在0.05,0.1,0.5 mg/kg添加水平下,两种待测农药的平均回收率为8 6％～110％;相对标准偏差(RSD)为1.5％～6.1％.结论:该方法高效简便、稳定性好、灵敏度高,适用于大米中氯虫苯甲酰胺和五氟磺草胺的检测.
Abstract
Objective:To establish a new QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the detection of chlorantraniliprole and penoxsulam residues in rice.Methods:After the sample was extracted with 0.2％formic acid-acetonitrile,purified with N-propylethylenediamine(PSA)and graphitized carbon black(GCB)packing,0.2％formic acid water and acetonitrile were used as mobile phases for gradient elution,and then subjected to C18 chromatography.UPLC-MS/MS was used to column separation and determination.Results:The limits of quantification(LOQ)of chlorantraniliprole and penoxsulam were both 0.004 mg/kg,and the method detection limits(LOD)were both 0.001 mg/kg.Chlorantraniliprole and penoxsulam had a good linear relationship in the range of 0.002～0.5 mg/L,and their coefficient was greater than 0.993.At the addition levels of 0.05,0.1,and 0.5 mg/kg,the average recovery rates of chlorantraniliprole and penoxsulam were 86％to 110％with the relative standard deviations(RSD)of 1.5％to 6.1％.Conclusion:This method is efficient and simple,has good stability and high sensitivity,and is suitable for the detection of chlorantraniliprole and penoxsulam in rice.
关键词
QuEChERS/氯虫苯甲酰胺/五氟磺草胺/大米/残留Key words
QuEChERS/chlorantraniliprole/penoxsulam/rice/residue引用本文复制引用
基金项目
怀化市科技计划创新项目(2021R3120)
湖南省教育厅科学研究项目(湘教通[2020]264号)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据