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1、南京医学院毕业论文摘要论文建立了蔬菜中 11 种农药多残留的气相色谱分析方法。对 NY/T761-2008蔬菜和水果中有机磷、有机氮、拟除虫菊酯和氨基甲酸酯类农药多残留的测定标准的蔬菜前处理方法进行了改进，探讨了蔬菜基质对检测的影响。使用 DB-17 毛细管柱分离，FPD检测器进行检测。结果显示：11 种有机磷农药分离效果好，在黄瓜、西红柿、生姜中的3 个浓度添加水平，回收率为 71.2%-117.9%，相对标准偏差（RSD）为 2.1%-11.2%，最低检出限为 0.005mg/kg-0.06mg/kg，保留时间为 6.396min-19.400min。在各自限性范围内线性关系好（r0.99
2、9）；使用 40加热氮吹浓缩，可分别提高敌敌畏、甲拌磷回收率至 95.00%和 103.3%；在被测得 13 种蔬菜中，甘蓝、娃娃菜、上海青有少量杂峰影响农药检出；韭菜有大量的基质峰干扰农药检出。为了有效控制蔬菜农药残留提供科学依据，2009 年 9 月至 12 月对天河区 4 家超市及 1 处农贸市场进行随机抽样检测，用气相色谱法测定其中的有机磷农药。共检测蔬菜样品 64 份，其中农药残留阳性的有 10 份，超标率为 15.63%。叶菜类蔬菜合格率为71.43%，而瓜菜类、根茎类和茄果类全部合格。在 11 种标的农药中，检测出 5 种，其中 3 种为国家禁用农药。论文还研究了不同清洗方法对去
3、除蔬菜中有机磷农药残留的影响。采用气相色谱法（GC）对经过不同方法浸泡处理的娃娃菜中敌敌畏和乐果的残留量进行分析，结果显示：除了超声波清洗之外，清水、洗涤剂以及食用碱均能不同程度的去除娃娃菜中残留的农药。其中斧牌洗洁精对敌敌畏和乐果两种农药残留的去除效果最佳，斧牌洗洁精对两种农药的去除率为分别为 84.38%和 76.11%。关键词：气相色谱（GC）；有机磷农药残留；蔬菜IIABSTRACTMethods were set up for determination of 11 organ phosphorus pesticides multi-residue in vegetables by
4、gas chromatography and define the scope of application of this method by analysis of vegetable matrix. Vegetable pretreatment method in standard of NY/T 761-2008 was modified in this paper, and DB-17 capillary column and flame photometric detector (FPD) were used. The result showed that 11 organ pho
5、sphorus pesticides were separated from each other. The fortified recovery of 11 pesticides gained from cucumber, tomato, and ginger with three spiked levels ranged from71.2% to 117.9%. The Relative standard deviation (RSD) was 2.1% to 11.2%, the Minimum detection limit of the method was 0.0050.06 mg
6、/kg for DB-17 column, and the Retention time was 6.396 to 19.400 minutes. The calibration curves showed good linearity with correlative coefficient of more than 0.999. Sample was heated up to 40 when blew by nitrogen (N2), the recoveries of Dichlorovos and Phorate would enhance to 95.00% and 103.3%
7、respectively. Among 13 vegetables detected, green pepper, baby cabbage and shanghai green have several peaks of matrix to impact detection of pesticide residues while garlic chive was found a large number of peaks interfere with the detection of pesticides.A survey of organ phosphorus pesticide in s
8、ixty four vegetable samples collected randomly from four supermarkets and one vegetable wholesale market of Guangzhou city was carried out from September to December in 2009. Gas chromatography analysis for 11 organ phosphorus pesticide residues in the samples showed that the qualification rate of l
9、eaf vegetables was 71.43%, and no investigated pesticide residue was detected in the all examined the raw melons vegetables, the root vegetables, and the solanaceous fruit vegetables. Five kinds of organ phosphorus pesticides were detected in 10 kinds of samples (64 samples) with the disqualificatio
10、n rate being of 15.63%, among which three prohibited pesticides for planting vegetables according to relevant laws were detected. Forbidden pesticide residue was detected with relatively high frequency in the vegetable samples.The effects of different rinsing methods on the removal ratio of organ ph
11、osphorus pesticide residues from Baby cabbage were investigated. The gas chromatography (GC) was used to analyze the pesticide residues in baby cabbage rinsed by different method. The results showed that clear water rinsing, detergent and edible alkali can remove the residual pesticide in baby cabba
12、ge at different level， except for treatment with ultrasonic. Among all these methods， detergent with brand of Axe can remove residual pesticide effectively. The removalratio of Dichlorovos and Dimethoate was 84.38%, 76.11% by detergent with brand of Axe.Keyword：Gas chromatography; organic phosphorus
13、 pesticide residue; vegetableVI目录摘要IAbstractII第一章：绪论11.1 有机磷农药11.2 蔬菜中有机磷农药残留现状21.3 农药残留危害41.3.1 农药残留对人体健康的危害41.3.2 农药残留对生态系统的危害51.3.3 农药对害虫天敌的危害51.3.4 农药对土壤微生物的危害51.3.5 农药对水环境的影响51.4 蔬菜中有机磷农药的前处理方法与分析方法61.4.1 农药残留的前处理技术61.4.2 农药残留的分析检测技术71.5 蔬菜表面有机磷农药的去除方法81.5.1 物理方法81.5.2 化学方法101.5.3 生物方法111.6 本研究
14、的目的与意义111.7 研究内容12第二章 蔬菜中 11 种有机磷农药残留的气相色谱检测及蔬菜基质影响的研究142.1 引言142.2 实验材料与仪器设备142.3 实验方法152.3.1 气相色谱分析条件152.3.2 GC-MS 分析条件162.3.3 样品提取162.3.4净化162.4 结果与讨论162.4.1 种有机磷农药混合标准液色谱分离效果图162.4.2 氮吹温度对敌敌畏、甲拌磷回收率的影响182.4.3 不同基质对检测效果的影响192.4.4 线性范围、标准曲线、检出限和保留时间232.4.5 回收率和精密度实验242.5 本章小节26第三章 广州市售蔬菜有机磷农药残留情况调
15、查分析273.1 引言273.2 实验材料与仪器设备273.3 实验方法273.3.1 测定方法273.3.2 评定标准283.4 结果与讨论283.4.1 总体检测情况283.4.2 不同种类农药检出率283.4.3 不同类别蔬菜中农药残留情况293.4.4 不同品种蔬菜中农药残留情况303.4.5 不同来源蔬菜的农药残留检测情况313.5 本章小节31第四章：清洗方法对蔬菜中有机磷农药残留去除效果的研究334.1 引言334.2 实验材料与仪器设备334.3 实验方法344.3.1 样品处理方法344.3.2 样品前处理方法344.3.3 GC 检测条件344.3.4 清洗方法344.3.5 农药残留率的计算354.4 结果与讨论354.4.1 清水浸泡时间对农药去除的效果354.4.2 超声波清洗对农药去除的效果364.4.3 洗涤剂浸泡对农药去除的效果374.4.4 食用碱浸泡对农药去除的效果394.5 本章小节40结论与展望41参考文献43第一章 绪论第一章绪论1.1 有机磷农药二十世纪末，在我国农药生产种类中，杀虫剂占了农药总产量的近 70%，而在杀虫剂总量中，有机磷农药又占了近 70%
