基于HPLC-UV-QDa检测不同剂型中噻唑膦和吡虫啉
Determination of fosthiazate and imidacloprid in variety formulations based on HPLC-UV-QDa
顾爱国 1陈昌旸 1刘凤琪 2李雪 3冯晨 1王胜录 1肖苏煜 1杨松4
作者信息
- 1. 江苏省产品质量监督检验研究院,南京 221111
- 2. 江苏省产品质量监督检验研究院,南京 221111;山东农业大学植物保护学院,山东泰安 271018
- 3. 江苏省产品质量监督检验研究院,南京 221111;长江大学农学院,湖北荆州 434000
- 4. 江苏省产品质量监督检验研究院,南京 221111;南京农业大学植物保护学院,南京 221111
- 折叠
摘要
建立了高效液相色谱-紫外检测器-质谱(HPLC-UV-QDa)测定5种不同剂型产品中噻唑膦和吡虫啉含量的分析方法.样品以乙腈+水(0.05％甲酸)为流动相,采用C18色谱柱进行梯度洗脱,结合紫外和质谱串联检测器进行定性和定量分析.研究结果显示,在质量浓度0.05～50 mg/L,噻唑膦、吡虫啉的线性关系良好,R2分别为0.999 2～0.999 9和0.999 1～0.999 6.在0.5、50、500 mg/kg等3个添加水平下,噻唑膦、吡虫啉的平均回收率分别为90.2％～103.9％和94.7％～104.1％,相对标准偏差(RSD)分别为1.04％～6.69％和1.27％～5.88％.噻唑膦和吡虫啉在5种基质中无明显基质效应,检出限分别为0.005和0.01 mg/L,定量限分别为0.02和0.04 mg/kg.方法灵敏度高、稳定性好、准确度高,适用于不同剂型产品中噻唑膦和吡虫啉的分析.
Abstract
A high performance liquid chromatography-ultraviolet detector-mass spectrometry(HPLC-UV-QDa)method was developed for the determination of fosthiazate and imidacloprid in 5 different formulations.The samples were analyzed by gradient elution separation,using acetonitrile-water(0.05％formic acid)as the mobile phase on C18 column.The results showed that the linear relations were good at the concentration of 0.05-50 mg/L,R2 of fosthiazate and imidacloprid were 0.999 2-0.999 9 and 0.999 1-0.999 6,respectively.Under the level of 0.5,50,500 mg/kg,the recoveries of fosthiazate and imidacloprid were 90.2％-103.9％and 94.7％-104.1％,and the relative standard deviations were 1.04％-6.69％and 1.27％-5.88％,respectively.The matrix effects of fosthiazate and imidacloprid were non-obvious in 5 typical substrates,and LOD were 0.005 and 0.01 mg/L,LOQ were 0.02 and 0.04 mg/kg.The method was suitable for the analysis of fosthiazate and imidacloprid in different formulations.
关键词
高效液相色谱-紫外检测器-质谱/噻唑膦/吡虫啉/基质效应/分析Key words
HPLC-UV-QDa/fosthiazate/imidacloprid/matrix effect/analysis引用本文复制引用
基金项目
江苏省农业科技自主创新项目(CX223017)
江苏省市场监督管理局科技计划项目(KJ2023011)
江苏省市场监督管理局科技计划重点研发项目(KJ2024003)
出版年
2024
NETL
NSTL
万方数据