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液相色谱食用菌种农药检测方法

时间:2018-05-06 09:36来源:毕业论文
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

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。
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 - 液相色谱食用菌种农药检测方法:http://www.751com.cn/huaxue/lunwen_14880.html
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