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气相色谱法测定农田土壤和水中烯啶虫胺残留
赵方方1, 林靖凌1, 谢德芳,等1
中国热带农业科学院分析测试中心 海南省热带果蔬产品质量安全重点实验室
摘要:
【目的】建立土壤和水中烯啶虫胺残留量的气相色谱检测方法。【方法】分别用2种方法对土壤和水中烯啶虫胺进行提取,从中选择操作性强的方法,并对实际土壤和水样品中烯啶虫胺残留的气相色谱测定条件进行优化。【结果】水体中乙腈和二氯甲烷提取的添加回收率分别为76.5%~87.6%,80.6%~92.7%,相差不大,但后者操作繁琐、耗时耗力,因此选择乙腈作提取剂;用丙酮 水(体积比2∶1)提取土壤样品,回收率远高于乙腈,其在土壤样品中的平均回收率为78.9%~81.0%,相对标准偏差为1.34%~2.65%。烯啶虫胺在水解过程中产生了新的物质,而在土壤降解中未出现影响农药定量的新物质,所以水样品中残留测定以优化后的色谱条件进行。本研究中气相色谱条件对烯啶虫胺的最小检出量为1×10-10 g,定量限为0.05 mg/kg。【结论】建立的检测方法灵敏度高,准确度高,线性好,符合农药残留分析要求,可用于土壤和水中烯啶虫胺残留量的测定。
关键词:  烯啶虫胺  土壤    气相色谱法
DOI:
分类号:
基金项目:中国热带农业科学院分析测试中心主任基金项目(2013-01);海南省自然科学基金项目(311060)
Measuring residues of nitenpyram in soil and water using GC
ZHAO Fang-fang,LIN Jing-ling,XIE De-fang,et al
Abstract:
【Objective】This study aimed to establish a method for determination of nitenpyram residues in soil and water using gas chromatography (GC).【Method】Two methods were used to extract nitenpyram from soil and water and the chromatographic conditions for the better one were optimized.【Result】Recoveries of nitenpyram in water with acetonitrile and dichloromethane were similar with values of 76.5%-87.6% and 80.6%-92.7%,respectively.Acetonitrile was chosen as extracting agent because the operation with dichloromethane was complex.Recoveries of nitenpyram in soil with acetone water (volume ratio 2∶1) as extracting agent were greater than the recoveries with acetonitrile and the average recoveries were 78.9%-81.0% and relative standard deviations were 1.34%-2.65%.New substance appeared during hydrolysis of nitenpyram,but no substance which could affect the quantification during the degradation in soil was found.The lowest detection limit of instrument for nitenpyram was 1×10-10 g,and the limit of quantitation was 0.05 mg/kg.【Conclusion】The established method with high sensitivity,high accuracy and good linearity met the requirement of pesticide residue analysis and could be used to detect nitenpyram in soil and water.
Key words:  nitenpyram  soil  water  GC method