摘要
采用水热法一步合成了氨基官能化MIL-101(Cr)金属骨架材料,将其作为注射泵辅助微固相萃取吸附剂,结合气相色谱-串联质谱检测,建立了稻米中6种有机磷农药的快速分离分析新方法。对前处理过程的条件进行优化,得到最优条件:材料用量5 mg、上样溶液pH=7.0,上样溶液盐浓度为5%NaCl,解吸溶剂丙酮的解吸体积为5 mL,最佳解吸速率0.7 mL/min。在最优条件下,6种有机磷农药在空白稻米样品中低中高三种添加浓度的回收率在83.0%-113.3%之间,日内日间相对标准偏差小于12.5%,表明所建立的方法具有良好的准确度和精密度。最后,将所建立的方法用于实际稻米样品中有机磷农药残留的分析,取得了很好的效果。
Organophosphorus pesticides(OPPs) are widely used in agricultural production.However, the safe issue of OPPs in food has also attracted more and more attention due to their high toxicity.In this paper, the amino-functionalized MIL-101(Cr) metal framework material was synthesized by hydrothermal reaction, and was used as adsorbent of syringe pump-assisted μ-SPE. Firstly, the adsorbent was loaded evenly on the organic filter membrane, and then the sample solution was driven by the injection pump to complete extraction through the adsorbent on the organic filter membrane.After the extraction, the sample was desorbed directly, avoiding the step of centrifugation in traditional dispersing μ-SPE,and greatly improving the speed of sample analysis.Lastly, the desorption solution was concentrated for detection by GC-MS/MS.From the above, a new method for rapid analysis of 6 OPPs in rice samples was established based on μ-SPE coupled with GC-MS/MS.Key parameters of syringe pump-assisted μ-SPE,including sample loading, cleaning and desorption solutions were optimized, and the optimal conditions were as following: 5 mg of the material dosage, the sample solution at pH 7 with 5% NaCl, the desorption rate of 0.7 mL/min, and the desorption volume of 5 mL.Under the optimized conditions, the method was evaluated according to recovery and precision.As a result, the recoveries of the six OPPs in the blank rice samples spiked at low, medium and high concentrations were 83.0%-113.3%,and inter-and intra-day relative standard deviations(RSDs) were less than 12.5%,indicating that the established method had good accuracy and precision.Finally, the established method was applied to the analysis of OPPs in actual rice sample, and satisfactory results were achieved.This study provided an effective method for the analysis of OPPs in rice.
作者
张隽娴
郑程
郑丹
刘丽
彭西甜
ZHANG Junxian;ZHENG Cheng;ZHENG Dan;LIU Li;PENG Xitian(Instituteof Agricultural Quality Standards and Testing Technology Research,Hubei Academy of Agricultural Science/Hubei Key Laboratory of Nutritional Quality and Safety of Agro products/Laboratory of Quality&Safety Risk Assessment for Agro-products(Wuhan),Ministry of Agriculture,Wuhan 430064)
出处
《分析科学学报》
CAS
CSCD
北大核心
2022年第5期561-567,共7页
Journal of Analytical Science
基金
湖北省自然科学基金重点研发计划项目(No.2020BBB078)。
