本文選題：韭菜　切入點(diǎn)：有機(jī)磷　出處：《湖南農(nóng)業(yè)大學(xué)》2015年碩士論文　論文類(lèi)型：學(xué)位論文

【摘要】：為控制韭菜中農(nóng)藥殘留,本文建立了韭菜中6種有機(jī)磷和6種煙堿類(lèi)兩類(lèi)農(nóng)藥的超高效液相色譜-串聯(lián)質(zhì)譜(UPLC-MS/MS)方法,通過(guò)殘留消解動(dòng)態(tài)和最終殘留試驗(yàn)研究吡蟲(chóng)啉在韭菜上的殘留行為。主要研究結(jié)果如下：建立了韭菜中6種有機(jī)磷農(nóng)藥的UPLC-MS/MS的檢測(cè)分析方法。樣品經(jīng)乙腈提取,石墨化炭黑固相萃取柱凈化,UPLC-MS/MS在多反應(yīng)離子監(jiān)測(cè)模式(MRM)下進(jìn)行檢測(cè),基質(zhì)匹配標(biāo)準(zhǔn)曲線定量。結(jié)果表明：6種農(nóng)藥均表現(xiàn)為基質(zhì)增強(qiáng)效應(yīng),在0.005、0.01 、0.05 mg/kg三個(gè)添加水平下,韭菜中6種農(nóng)藥的平均回收率為69.1%～110.4%；相對(duì)標(biāo)準(zhǔn)偏差(RSD,n=5)為2.2%～19.1%;在韭菜基質(zhì)中檢出限LOD為0.003 ng,最低檢出濃度(LOQ)為0.005 mg/kg,試驗(yàn)結(jié)果均符合農(nóng)藥殘留分析方法要求,該方法簡(jiǎn)單、快速、高效,適用于韭菜中農(nóng)藥殘留檢測(cè)。利用建立方法對(duì)市場(chǎng)韭菜進(jìn)行檢測(cè),甲胺磷、對(duì)硫磷、甲基對(duì)硫磷、辛硫磷均未檢出；甲拌磷的殘留量為0.005～0.087 mg/kg;毒死蜱的殘留量為0.005～0.171 mg/kg。建立了韭菜中6種煙堿類(lèi)農(nóng)藥UPLC-MS/MS的檢測(cè)分析方法。樣品經(jīng)乙腈提取,分散固相萃取凈化(GCB 10 mg, PSA 50 mg, C18 50 mg, MgSO4 50 mg),利用UPLC-MS/MS在多反應(yīng)離子監(jiān)測(cè)模式(MRM)下進(jìn)行檢測(cè),基質(zhì)匹配標(biāo)準(zhǔn)曲線定量。結(jié)果表明：6種農(nóng)藥均表現(xiàn)為基質(zhì)增強(qiáng)效應(yīng)；在0.005、0.01、0.05 mg/kg三個(gè)添加水平下,6種新煙堿類(lèi)農(nóng)藥的平均回收率為73.5%～101.3%,相對(duì)標(biāo)準(zhǔn)偏差(RSD,n=5)為1.1%-8.6%,在韭菜基質(zhì)中檢出限LOD為0.003 ng,最低檢出濃度(LOQ)為0.005 mg/kg,試驗(yàn)結(jié)果均符合農(nóng)藥殘留分析要求,該方法簡(jiǎn)單、快速、高效,適用于韭菜中農(nóng)藥殘留檢測(cè)。建立土壤中吡蟲(chóng)啉的UPLC-MS/MS檢測(cè)分析方法。樣品經(jīng)乙腈提取,分散固相萃取凈化(PSA 50 mg, C18 50 mg, MgSO4 100 mg),利用UPLC-MS/MS在多反應(yīng)離子監(jiān)測(cè)模式(MRM)下進(jìn)行檢測(cè),基質(zhì)匹配標(biāo)準(zhǔn)曲線定量。結(jié)果表明：在0.005、0.01、0.05 mg/kg三個(gè)添加水平下,吡蟲(chóng)啉在土壤中的平均回收率為86.2%-93.9%,相對(duì)標(biāo)準(zhǔn)偏差(RSD,n=5) 2.5%～7.9%;吡蟲(chóng)啉在土壤中檢出限LOD為0.003 ng;吡蟲(chóng)啉在土壤中定量限LOQ為0.005 mg/kg,準(zhǔn)確度、精密度符合農(nóng)藥殘留分析方法的要求,該方法適用于土壤樣品中吡蟲(chóng)啉殘留檢測(cè)。于2014年在山東進(jìn)行了吡蟲(chóng)啉在韭菜上的消解動(dòng)態(tài)和最終殘留試驗(yàn)。消解動(dòng)態(tài)試驗(yàn)結(jié)果表明：吡蟲(chóng)啉在韭菜和土壤中的消解符合一級(jí)動(dòng)力學(xué)方程,分別為Ct=0.434e-0-362t和Ct=1.6234e-0.183t,相關(guān)系數(shù)(r)為0.978和0.906,在韭菜和土壤中的殘留消解半衰期分別為1.9 d和3.8 d。吡蟲(chóng)啉10%顆粒劑按有效濃度225 g a.i/hm2和337.5 g a.i/hm2灌根1-2次(施藥間隔期為7 d)進(jìn)行最終殘留試驗(yàn)。最終殘留試驗(yàn)結(jié)果表明：距最后一次施藥后的14d時(shí),吡蟲(chóng)啉在韭菜中最終殘留量低于0.017 mg/kg,在土壤中的最終殘留范圍0.054～0.157 mg/kg。故提出吡蟲(chóng)啉在韭菜中安全合理使用建議：按最高制劑用藥量337.5 g a.i/hm2,最多施藥2次,施藥間隔期為7 d,安全間隔期為14 d。
[Abstract]:In order to control pesticide residues in Chinese chives, a high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method was developed for the control of six organophosphorus and six nicotine pesticides in Chinese chives. The residual behavior of imidacloprid on leek was studied by residue digestion dynamics and final residue test. The main results were as follows: a method for the determination and analysis of six organophosphorus pesticides in leek was established. The samples were extracted by acetonitrile. UPLC-MS / MS was detected on a graphitized carbon black solid phase extraction column under a multi-reaction ion monitoring model. The matrix matching standard curve was quantified. The results showed that all of the 6 pesticides showed matrix enhancement effect, and at the three additive levels of 0.005 ~ 0.01 ~ 0.05-0. 05 mg/kg, The average recovery of 6 pesticides in leek was 69.1 mg / kg; the relative standard deviation (RSD) was 2.2 / 19.1.The detection limit was 0.003 ng / kg and the lowest detectable concentration (LOQ) was 0.005 mg / kg in leek matrix. The results of the test were all in accordance with the requirements of pesticide residue analysis method. The method was simple, rapid and efficient, and the detection limit was 0.003 ng / kg, and the lowest detectable concentration was 0.005 mg / kg. It is suitable for the determination of pesticide residues in leek. Methamidophos, parathion, methyl parathion and phoxim were not detected by the established method. The residues of phorate and chlorpyrifos were 0.005N 0.087 mg / kg and 0.005N 0.171 mg / kg respectively. A method for the determination and analysis of six niacin pesticides UPLC-MS/MS in leek was established. The samples were extracted by acetonitrile. GCB10 mg, PSA 50 mg, C18 50 mg, MgSO4 50 mg were purified by dispersive solid phase extraction (SPE). The results showed that the matrix matching standard curve was quantitative by using UPLC-MS/MS in multi-reaction ion monitoring mode. The results showed that all of the 6 pesticides showed matrix enhancement effect. The average recoveries of six new nicotine pesticides were 73.5 mg / kg, RSD = 1.1-8.6mg / kg, LOD = 0.003 ng / kg and LOQ = 0.005 mg / kg in Chinese chive matrix, respectively. The average recovery rate of six new nicotine pesticides was 73.5 mg / kg. The results met the requirements of pesticide residue analysis, and the relative standard deviation (RSD) was 1.1- 8.6mg / kg, and the detection limit was 0.003 ng / kg and the lowest detectable concentration was 0.005 mg / kg in leek matrix, and the average recovery rate of six new nicotine pesticides was 73.5 mg / kg, and the relative standard deviation (RSD) was 1.1-8.6%. The method is simple, rapid, efficient and suitable for the determination of pesticide residues in leek. A UPLC-MS/MS method for determination of imidacloprid in soil was established. The sample was extracted by acetonitrile. PSA50 mg, C18 50 mg, MgSO4 100 mg / L were purified by dispersive solid phase extraction (SPE). The results showed that the matrix matching standard curve was determined by using UPLC-MS/MS under the multi-reaction ion monitoring mode. The results showed that the results showed that at the three addition levels of 0.005mg, C1850mgand MgSO4 100mgg, the results showed that, The average recovery of imidacloprid in soil was 86.2% -93.9 with relative standard deviation (RSD) 2.5% and 7.9%; the detection limit of imidacloprid in soil was 0.003 ng / kg; the quantitative limit of imidacloprid in soil was 0.005 mg / kg / kg; the accuracy and precision of imidacloprid was 0.005 mg / kg / kg, and the accuracy and precision of imidacloprid met the requirements of pesticide residue analysis. This method is suitable for the determination of imidacloprid residues in soil samples. In 2014, the degradation dynamics and final residues of imidacloprid on leek were carried out in Shandong Province. The results showed that imidacloprid in leek and soil. The solution accords with the first-order kinetic equation, The correlation coefficient (r) was 0.978 and 0.906, respectively. The half-life of residual digestion in leek and soil was 1.9 d and 3.8 days, respectively. Imidacloprid 10% granules were irrigated with 225g a.i / ha and 337.5 g a.i / hm ~ 2 at effective concentration for 1-2 times (the interval period was 7 days). The final residue test was carried out. The results of the final residue test showed that: 14 days after the last application, The final residue of imidacloprid in leek was less than 0.017 mg / kg, and the final residue range in soil was 0.054 ~ 0.157 mg / kg. Therefore, the safe and reasonable use of imidacloprid in leek was suggested: the maximum dosage of imidacloprid in leek was 337.5 g. The application interval was 7 days and the safe interval was 14 days.
【學(xué)位授予單位】：湖南農(nóng)業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：X592

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