氨基功能化石墨烯固相微萃取-气相色谱法测定水样中7种有机磷农药残留量
目的 建立氨基功能化石墨烯固相微萃取-气相色谱法同时测定水样中7种有机磷农药残留(硫线磷、地虫硫磷、氯唑磷、甲基毒死蜱、磷胺、喹硫磷和苯线磷)。方法 水样中残留的有机磷农药用25 mg氨基功能化石墨烯富集, 用6 mL丙酮洗脱, 然后使用气相色谱-火焰光度检测器(gas chromatography-flame photometric detector, GC-FPD)测定。对气相色谱条件和影响萃取效率的多种因素进行优化。结果 在优化的条件下, 7种有机磷农药标准曲线线性关系良好, 线性系数为0.9905~0.9988, 检出限为0.025~0.04 μg/L, 定量限为0.08~0.12 μg/L。氨基功能化石墨烯对7种有机磷农药的富集倍数为183倍~307倍, 萃取率为45.8%~76.8%, 3个浓度添加水平(1、5.0、50 μg/L)的加标平均回收率在70.0%~105%, 相对标准偏差为7.98%~14.5%。结论 该方法具有操作简单, 快速、准确度和灵敏度高、试剂用量少等特点, 适用于水样中 7种有机磷农药残留量的测定。
Objective To establish a method for determination of 7 organophosphorus pesticides (cadusafos, fonofos, isazofos, chlorpyrifos-methyl, phosphamidon, quinalphos and fenamiphos) in water by-NH2 functionalized graphene solid phase micro extraction-gas chromatography. Methods The organophosphorus pesticides remaining in the water samples were enriched with 25 mg amino functionalized graphene, eluted with 6 mL acetone, and determined by gas chromatography-flame photometric detector (GC-FPD), and then gas chromatographic conditions and various factors affecting extraction efficiency were optimized. Results Under the optimum conditions, the standard curves of 7 organophosphorus pesticides had good linearity, and the correlation coefficients were 0.9905?0.9988. The limits of detection were 0.025?0.04 μg/mL, and the limits of quantitation were 0.08?0.12 μg/L. The enrichment factors (EF) of 7 organophosphorus pesticides were 183?307, and extraction rates were 45.8%?76.8%. The average recoveries of 3 spiked levels (1, 5.0, and 50 μg/L) were 70.0%?105%, and the relative standard deviations were 7.98%?14.5%. Conclusion The established method has the advantages of simply, rapidity, high accuracy and sensitivity, and less reagent consumption, which is suitable for the determination of 7 organphosphorus pesticide residues in water samples.
标题：氨基功能化石墨烯固相微萃取-气相色谱法测定水样中7种有机磷农药残留量
英文标题：Determination of 7 organophosphorus pesticide residues in water by -NH2 functionalized graphene solid phase micro extraction-gas chromatography
作者：
耿慧春 云南省农业科学院质量标准与检测技术研究所；农业农村部农产品质量监督检验测试中心(昆明)
梅文泉 云南省农业科学院质量标准与检测技术研究所；农业农村部农产品质量监督检验测试中心(昆明)
王正伟 云南省镇沅县农业环境监测站
方海仙 云南省农业科学院质量标准与检测技术研究所；农业农村部农产品质量监督检验测试中心(昆明)
陈兴连 云南省农业科学院质量标准与检测技术研究所；农业农村部农产品质量监督检验测试中心(昆明)
王丽 云南省农业科学院质量标准与检测技术研究所；农业农村部农产品质量监督检验测试中心(昆明)
汪禄祥 云南省农业科学院质量标准与检测技术研究所；农业农村部农产品质量监督检验测试中心(昆明)
中文关键词:氨基功能化石墨烯,固相微萃取,气相色谱法,有机磷,农药残留,水样,
英文关键词:-NH2 functionalized graphene,solid phase micro extraction,gas chromatography,organophosphorus,pesticide residues,water sample,
发表日期：2019-03-29
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