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作 者:方海仙[1,2] 毕嘉蕊 耿慧春 梅文泉[1,2] FANG Hai-Xian;BI Jia-Rui;GENG Hui-Chun;MEI Wen-Quan(Quality Standardizing and Testing Technology Institute,Yunnan Academy of Agricultural Sciences,Kunming 650205,China;Supervision&Testing Center for Farm Products Quality,Ministry of Agriculture and Rural Affairs(Kunming Section),Kunming 650205,China;Agricultural Products Quality and Safety Inspection and Monitoring Station of Linxiang District,Lincang 677000,China)
机构地区:[1]云南省农业科学院质量标准与检测技术研究所,昆明650205 [2]农业农村部农产品质量监督检验测试中心(昆明),昆明650205 [3]临沧市临翔区农产品质量安全检验检测站,临沧677000
出 处:《食品安全质量检测学报》2021年第2期623-628,共6页Journal of Food Safety and Quality
基 金:云南省科技计划青年基金(2018FD126);云南省重点研发计划(2018BC005,2019ZG001)。
摘 要:目的建立QuEChERS-气相色谱法测定葡萄酒中6种杀虫剂残留的分析方法。方法样品经乙腈提取后,提取液采用QuEChERS前处理后上机测定。优化的色谱条件为:DB-1石英毛细管柱(0.53 mm×1.50μm,30m),采用程序升温分离,火焰光度检测器检测,采用外标法定量。结果在优化的条件下,6种杀虫剂在0.01~1.50μg/mL范围内线性良好,相关系数(r)均大于0.999,定量限为0.02~0.025 mg/kg, 6种杀虫剂平均回收率为81%~115%,相对标准偏差(relative standard deviation, RSD)在0.870%~7.29%(n=3)之间。结论该方法具有操作简便、快速、准确的特点,适用于葡萄酒中6种杀虫剂残留痕量分析。Objective To establish a method for the determination of 6 insecticides in wine by gas chromatography combined with QuEChERS. Methods After extracted with acetonitrile, the sample extract was pretreated by QuEChERS method. Under the optimized chromatographic conditions, the analysis was carried out with a capillary column(DB-1, 0.53 mm×1.50 μm, 30 m), monitoring with an flame-photometric detector, the 6 insecticides were separated by temperature-programming of the column. External standard method was used for quantitative analysis. Results Under the optimized conditions, good linearities were obtained in the range of 0.01-1.50 μg/mL for 6 insecticides with the correlation coefficients greater than 0.999 by external method, the limits of quantification of the method were 0.02 mg/kg to 0.025 mg/kg. The average recoveries of the six kinds of insecticide ranged from 81% to 115% with the relative standard deviations(RSDs) from 0.870% to 7.29%. Conclusions The method is simple, rapid and accurate, and can be used for the routine analysis of 6 insecticides residues in wine.
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