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摘要: 本课题研究了食用菌种农药多残留检测方法，并主要研究了新烟碱类杀虫剂啶虫脒的仪器方法和检测条件等。为此做了两部分实验。
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第一部分是农药多残留的检测方法。利用液相色谱质谱联用仪测样品其农药残留情况。液相色谱串联质谱采用的是EC-C18色谱柱（3.0×100mm；2.7um），其中液相色谱条件：流动相A甲醇，B为1:9=甲醇：水（0.05%甲醇，5mmol/l醋酸铵）；流速为0.3ml/min；梯度洗脱0～1min，10%B；1～5min，10%～90%B；5～9.5min，90%B；9.5-9.6min，90%～10%B；9.6～12min，10%B；柱温40℃，进样量5ul。质谱条件：电喷雾电离源（ESI），正离子模式。经测定样品中含有咪鲜胺、多菌灵等农药。22313
第二部分是研究单一农药啶虫脒的测定条件及方法。仪器方法是在流动相甲醇：水=20:80，检测波长为246nm。添加回收实验中称取15g未检测含有啶虫脒的双孢菇，做了三组平行试验，预处理方法和多残留检测的一样，只不过是在双孢菇中添加浓度为400ppm的啶虫脒标准品0.1ml，所用的仪器是高效液相色谱仪，仪器条件为啶虫脒仪器条件，得到的回收率为分别104%、106%、108%，标准偏差为2.0%。说明该种方法检测啶虫脒的效果较好。另外探究了啶虫脒的提取剂的选择性，综合情况考虑乙腈比较合适。
毕业论文关键字：啶虫脒；液相色谱；食用菌；多残留检测液；相色谱质谱联用
Abstct:
The research of pesticide residues in edible fungi species detection methods and studies the neonicotinoids acetamiprid methods and instruments to detect conditions. Done a two-part test.
The first part is a pesticide residue detection method. By liquid chromatography mass spectrometry test sample which pesticide residues. Liquid chromatography-tandem mass spectrometry is used in EC-C18 column (3.0 × 100mm; 2.7um), wherein the liquid chromatography conditions: mobile phase A methanol , B = 1:9 methanol: water ( 0.05% methanol , 5mmol / l ammonium acetate ) ; flow rate of 0.3ml/min; gradient elution 0 ~ 1min, 10% B; 1 ~ 5min, 10% ~ 90% B; 5 ~ 9.5min, 90% B; 9.5-9.6min, 90% ~ 10% B; 9.6 ~ 12min, 10% B; column temperature was 40 ℃, injection volume 5ul. MS conditions : electrospray ionization (ESI), the positive ion mode . The determination of samples containing prochloraz, carbendazim and other pesticides .
The second part is the study of a single pesticide acetamiprid measurement conditions and methods. Instrument approach is in the mobile phase of methanol : water = 20:80 , detection wavelength of 246nm. Add recycling experiment weighed 15g white button mushrooms contain acetamiprid undetected, do three sets of parallel experiments , the same pretreatment methods and multi-residue testing, but is added to a concentration of 400ppm of Agaricus acetamiprid Standard 0.1 ml, is used in high performance liquid chromatography instrument , instrument conditions as acetamiprid instrument conditions , the recoveries obtained were 104% , 106% , 108%, a standard deviation of 2.0%. Description of the methods to detect acetamiprid better. Also explore the selective extraction of acetamiprid agent, consider the consolidation of acetonitrile appropriate.
Key Words: Acetamiprid; liquid chromatography; liquid chromatography mass spectrometry; mushroom.
目 录 I
1 前言 - 1 -
1.1 选题依据 - 1 -
1.2 农药的发展历程 - 1 -
1.3 新烟碱类杀虫剂的抗性及治理 - 1 -
1.4新烟碱类杀虫剂的发展趋势 - 2 -
1.5 农药的环境行为和环境效应 - 2 -
1.5.1环境行为 - 2 -
1.6文献综述 - 2 -
1.7 现代农药残留检测仪器分析方法 - 3 -
1.7.1 气相色谱法(GC) - 3 -