本文選題：蘋果 + 葉片��； 參考：《農(nóng)藥學(xué)學(xué)報》2016年06期

【摘要】：為了解吡唑醚菌酯在蘋果葉片中的殘留動態(tài),合理評估其持效期,比較了液液萃取、固相萃取以及Qu ECh ERS(Quick、Easy、Cheap、Effective、Rugged、safe)3種樣品前處理方法對蘋果葉片中吡唑醚菌酯添加回收率的影響,優(yōu)化了基于超高效液相色譜-串聯(lián)質(zhì)譜(UPLCMS/MS)的檢測條件與方法。結(jié)果表明:采用Qu ECh ERS法提取時回收率較高,所需有機(jī)溶劑少,時間短,重復(fù)性好,適合蘋果葉片中吡唑醚菌酯的萃取和凈化;對于蘋果葉片,萃取和凈化步驟中的填料可減少為乙二胺-N-丙基甲硅烷(PSA)和石墨化碳黑(GCB)2種,其最佳用量PSA為0.025 g/m L,GCB為0.020 g/m L;蘋果葉組織對樣品檢測具有微弱的基質(zhì)增強(qiáng)效應(yīng)。通過對Qu ECh ERS方法的改進(jìn)以及對色譜-質(zhì)譜檢測參數(shù)的優(yōu)化,建立了蘋果葉片中吡唑醚菌酯殘留的檢測方法,該方法的線性范圍為0.01~50.0 mg/L,定量限為0.01 mg/kg。在0.01~10 mg/kg4個添加水平下,吡唑醚菌酯在蘋果葉片中的回收率為92%~99%,相對標(biāo)準(zhǔn)偏差為2.2%~5.3%。田間實(shí)測結(jié)果表明:蘋果葉片噴施1 000 mg/L的25%吡唑醚菌酯乳油,其殘留消解動態(tài)符合一級反應(yīng)動力學(xué)模型c_t=79.87 e~( 0.053 3 t),半衰期為13 d。
[Abstract]:In order to understand the residual dynamics of pyrazole in apple leaves and evaluate its retention period reasonably, the effects of liquid-liquid extraction, solid phase extraction and QUECH ERSX QY EasyEY Effective Effective RuggedSafeto on the recovery of pyrazole in apple leaves were compared. The detection conditions and methods based on ultra high performance liquid chromatography-tandem mass spectrometry (UPLCs / MS) were optimized. The results show that the recovery rate is high, the organic solvent is less, the time is short and the repeatability is good, which is suitable for the extraction and purification of pyrazole in apple leaves. In the extraction and purification process, the fillers can be reduced to ethylenediamine-N-propylmethylsilane (PSAs) and graphitized carbon black (GCBs), the optimum dosage of which is 0.025 g / m ~ (-1) GCB = 0.020 g / m ~ (L), and apple leaf has a weak matrix enhancement effect on sample detection. By improving the QU ECh ERS method and optimizing the detection parameters of the chromatography-mass spectrometry, a method for the determination of pyrazolyl ester residues in apple leaves was established. The linear range of the method was 0.01 ~ 50.0 mg / L, and the quantitative limit was 0.01 mg / kg 路L ~ (-1). The recovery rate of pyrazole in apple leaves was 92 and the relative standard deviation was 2.2 / 5.3under the addition level of 0.01 ~ 10 mg/kg4. The field test results showed that the residual digestion kinetics of apple leaves sprayed with 25% Pyrazolyl Ester EC of 1 000 mg / L was consistent with the first-order reaction kinetics model c_t=79.87 (0.053 3 t ~ (-1) with a half-life of 13 days.
【作者單位】： 青島農(nóng)業(yè)大學(xué)農(nóng)學(xué)與植物保護(hù)學(xué)院/山東省植物病蟲害綜合防控重點(diǎn)實(shí)驗(yàn)室;
【基金】：現(xiàn)代農(nóng)業(yè)產(chǎn)業(yè)技術(shù)體系(CARS-28) 山東省泰山學(xué)者建設(shè)工程專項資助經(jīng)費(fèi)
【分類號】：S481.8;O657.63

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