甜菜中多种农药残留联合测定方法研究及风险分析

【作者】 刘琳；

【导师】 王皙玮； 周芹； 殷博；

【作者基本信息】 黑龙江大学 ， 农业硕士（专业学位）， 2022， 硕士

【摘要】 甜菜是重要的糖料作物之一,在其生长过程中会使用各种农药进行病虫草害防治,这些农药如果使用不当,将会对环境和人类健康造成一定的危害风险。目前,国内外对于甜菜中农药残留分析的研究报道较少,因此建立简单、快速、灵敏的多农药残留分析技术是保障甜菜食品安全的关键,也是相关科研工作的研究重点。本论文建立了两项甜菜中多农药残留的联合测定方法,并应用到甜菜主产区实际样品的风险分析中。研究的主要内容和结果如下:1.建立了改良的Qu ECh ERS法结合气相色谱-电子捕获检测器(GC-ECD)用于红甜菜中20种农药残留的联合测定方法。分别考察了色谱的程序升温条件、提取溶剂、净化方法对检测结果的影响。在优化的色谱条件和前处理条件下,20种农药线性关系良好(R~2>0.99),检出限为0.12μg/kg～0.063 mg/kg,平均回收率为62.0%～116.5%,相对标准偏差为1.9%～10.9%。该方法准确、高效、重复性好,适用于甜菜中有机氯、拟除虫菊酯类多农药残留分析。2.利用气相色谱-火焰光度检测器(GC-FPD),建立了甜菜中15种有机磷农药残留的联合测定方法,可适用于糖用甜菜、食用甜菜(红甜菜)及叶用甜菜中农药多残留的测定。分别考察了色谱的程序升温条件、提取温度、净化方法对检测结果的影响。在优化的色谱条件和前处理条件下,15种农药线性关系良好(R~2>0.99),检出限为0.0047 mg/kg～0.0261 mg/kg,平均回收率为60.3%～120%,相对标准偏差为2.0%～19.3%。该方法操作简单、分析时间短、有机溶剂用量少,适用于甜菜中有机磷多农药残留分析。3.利用建立的GC-ECD和GC-FPD测定方法分别对我国三大甜菜主产区的208个糖甜菜样品进行农药残留检测,并对其进行风险分析,具备参考值的检出农药均未超标,慢性膳食摄入风险商均小于100%,表明甜菜中农药对人体健康危害风险较低。更多还原

【Abstract】 Sugar beet is one of the important sugar crops,and a variety of pesticides are used to control diseases,pests and weeds during its growth.If these pesticides are used improperly,they will pose a certain risk of harm to the environment and human health.At present,there are few research reports on the analysis of pesticide residues in sugar beet at home and abroad.Therefore,establishing a simple,fast and sensitive analysis technology for multi-pesticide residue is the key to ensuring the food safety of sugar beet,and it is also the focus of related scientific research work.In this paper,two methods for the combined determination of multi-pesticide residues in sugar beet will be established and applied to the risk analysis of actual samples in the main sugar beet producing areas.The following are the main contents and results of the research:1.An improved Qu ECh ERS method combined with gas chromatography-electron capture detector(GC-ECD)was established for the combined determination of 20pesticide residues in red beet.The effects of temperature-programmed conditions,extraction solvents,and purification methods of chromatography on the detection results were investigated respectively.Under the optimized chromatographic conditions and pretreatment conditions,20 pesticides had a good linear relationship(R~2>0.99),the limits of detection were 0.12μg/kg～0.063 mg/kg,the average recoveries were62.0%～116.5%,and the relative standard deviations were 1.9%～10.9%.The method is accurate,efficient and reproducible.It is suitable for the analysis of various organochlorine and pyrethroid pesticide residues in sugar beet.2.A method with gas chromatography-flame photometric detector(GC-FPD)was established for the combined determination of 15 organophosphorus pesticide residues,which can be applied to the determination of pesticide residues in sugar beet,table beet(red beet)and leaf beet.The effects of temperature-programmed conditions,extraction temperature,and purification methods of gas chromatography on the detection results were investigated respectively.Under the optimized chromatographic conditions and pretreatment conditions,15 pesticides had a good linear relationship(R~2>0.99),the limits of detection were 0.0047 mg/kg～0.0261 mg/kg,the average recoveries were60.3%～120%,and the relative standard deviations were 2.0%～19.3%.The method has simple operation,short analysis time and less organic solvent consumption.It is suitable for the analysis of various organophosphorus residues in sugar beet.3.The established GC-ECD and GC-FPD analysis methods were used to detect pesticide residues in 208 sugar beet samples from three major sugar beet producing areas in China.Then I analyzed the risk of pesticide residues in sugar beets according to the detection results,the detected pesticides with reference values did not exceed the standard.The chronic dietary intake risk quotients were all less than 100%,indicating that pesticides in sugar beets have a low risk of harm to human health.更多还原