【摘要】：研究目的：建立尿液中馬拉硫磷3種代謝產(chǎn)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）和滅多威的固相萃取-氣相色譜/質(zhì)譜聯(lián)用（SPE-GS/MS）快速定性定量的分析方法，并利用該方法對大鼠尿液中馬拉硫磷3種代謝產(chǎn)物、滅多威進行了研究。 研究方法：以空白尿樣加磷酸二甲酯、二甲基硫代磷酸酯、二甲基二硫代磷酸酯及滅多威標準品，對尿樣進行前處理方法、氣相色譜-質(zhì)譜條件、回收率、特異性、精密度、檢出限、穩(wěn)定性進行全面考察，建立SPE-GS/MC快速定性定量分析方法： 采用SPE-GS/MS法：在一定的條件下測定不同時間段內(nèi)大鼠尿液中馬拉硫磷3種代謝產(chǎn)物和滅多威的濃度。并同時測定不同時間段內(nèi)大鼠尿肌酐的含量，進行校準待測物質(zhì)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，并對24h內(nèi)對各組大鼠尿液中馬拉硫磷3種代謝產(chǎn)物、滅多威各自的濃度變化進行描述。 研究結(jié)果：馬拉硫磷3種代謝產(chǎn)物和滅多威在11.2min內(nèi)得到良好分離，DMP、DMTP、DMDTP、滅多威的保留時間（min）分別是：4.632、4.858、7.275、6.039。加標回收率大于87.9%,相對標準偏差小于8.9%,樣品-20℃放置2周后相對偏差小于9.4%,DMP、DMTP、DMDTP、滅多威大鼠尿液中的最低檢出濃度分別為3.0、0.30、4.0、0.4μg/ml（S/N=3），并在灌胃后在不同時間段內(nèi)檢測到3種代謝產(chǎn)物、滅多威。 研究結(jié)論：所建立的分析方法簡單、準確、快速、靈敏,具有較好的實驗重復性，是一種簡單的凈化提取和準確可靠的氣相色譜質(zhì)譜檢測方法,可對大鼠尿液中馬拉硫磷3種代謝產(chǎn)物及滅多威進行定性定量的檢測，為應用于職業(yè)暴露人群馬拉硫磷、滅多威、馬拉硫磷滅多威混配農(nóng)藥接觸水平的檢測提供了參考。
[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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