马拉硫磷、灭多威混配制剂生物标志物测定方法的研究

发布时间：2018-10-09 18:50

【摘要】：研究目的：建立尿液中马拉硫磷3种代谢产物磷酸二甲酯（imethylphosphate DMP）、二甲基硫代磷酸酯（Dimethyl thiophosphrate DMTP）、二甲基二硫代磷酸酯（Dimethyl dithiophosphrate DMDTP）和灭多威的固相萃取-气相色谱/质谱联用（SPE-GS/MS）快速定性定量的分析方法，并利用该方法对大鼠尿液中马拉硫磷3种代谢产物、灭多威进行了研究。 研究方法：以空白尿样加磷酸二甲酯、二甲基硫代磷酸酯、二甲基二硫代磷酸酯及灭多威标准品，对尿样进行前处理方法、气相色谱-质谱条件、回收率、特异性、精密度、检出限、稳定性进行全面考察，建立SPE-GS/MC快速定性定量分析方法： 采用SPE-GS/MS法：在一定的条件下测定不同时间段内大鼠尿液中马拉硫磷3种代谢产物和灭多威的浓度。并同时测定不同时间段内大鼠尿肌酐的含量，进行校准待测物质含量。大鼠灌胃后，收集0.5h，1h，2h，3h，6h，9h，，12h，15h，18h，21h，24h的全部大鼠尿，并对24h内对各组大鼠尿液中马拉硫磷3种代谢产物、灭多威各自的浓度变化进行描述。 研究结果：马拉硫磷3种代谢产物和灭多威在11.2min内得到良好分离，DMP、DMTP、DMDTP、灭多威的保留时间（min）分别是：4.632、4.858、7.275、6.039。加标回收率大于87.9%,相对标准偏差小于8.9%,样品-20℃放置2周后相对偏差小于9.4%,DMP、DMTP、DMDTP、灭多威大鼠尿液中的最低检出浓度分别为3.0、0.30、4.0、0.4μg/ml（S/N=3），并在灌胃后在不同时间段内检测到3种代谢产物、灭多威。 研究结论：所建立的分析方法简单、准确、快速、灵敏,具有较好的实验重复性，是一种简单的净化提取和准确可靠的气相色谱质谱检测方法,可对大鼠尿液中马拉硫磷3种代谢产物及灭多威进行定性定量的检测，为应用于职业暴露人群马拉硫磷、灭多威、马拉硫磷灭多威混配农药接触水平的检测提供了参考。
[Abstract]:Objective: to establish a solid phase extraction-gas chromatography-mass spectrometry (SPE-GS/MS) method for the determination of three metabolites of malathion, dimethyl phosphate (imethylphosphate DMP), dimethyl thiophosphate (Dimethyl thiophosphrate DMTP), dimethyl dithiophosphate (Dimethyl dithiophosphrate DMDTP) and methomyl dithiophosphate (SPE-GS/MS) in urine. Rapid qualitative and quantitative analysis, Three metabolites of malathion in rat urine, methomyl, were studied by this method. Methods: urine samples were pretreated with dimethyl phosphate, dimethyl thiophosphate, dimethyl dithiophosphate and methomyl dithioate, gas chromatography-mass spectrometry (GC-MS), recovery, specificity and precision. The detection limit and stability were investigated and the rapid qualitative and quantitative analysis method of SPE-GS/MC was established. The method of SPE-GS/MS was used to determine the concentration of malathion and methomyl in rat urine under certain conditions. At the same time, the content of creatinine in urine of rats was measured in different time periods, and the content of substances to be measured was calibrated. After the rats were perfused by stomach, all the urine samples of rats were collected from the urine samples of rats at 0.5 h ~ 1 h ~ 2 h ~ 3 h ~ 6 h ~ 9 h ~ (12) h ~ (18) ~ 21 h ~ (-1) ~ 24 h, and the concentrations of malathion metabolites and methomyl in the urine of each group were described within 24 h. The results showed that three metabolites of malathion and methomyl were well separated in 11.2min. The retention time (min) of methomyl was 4.632n4.8587.2756.039. The recoveries were greater than 87.9, the relative standard deviations were less than 8.9, the relative deviations of samples were less than 9.4% after being placed at -20 鈩

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