摘要
建立了固相萃取前处理技术结合气相色谱-串联质谱法同时测定六堡茶中52种农药残留量的快速检测方法。样品粉碎后,过筛,称取2.0 g样品,加入乙腈超声提取后,将提取液浓缩至2.0 mL,再经石墨化碳黑氨基复合固相萃取柱净化,净化液用气相色谱-串联质谱法分析,采用空白基质液配制标准曲线,内标法进行定量分析。结果表明,52种农药残留目标物在0.005~0.500μg·mL-1时线性关系良好,相关系数均大于0.995。方法检出限为0.002~0.030 mg·kg^(-1),定量限为0.004~0.060 mg·kg^(-1)。在0.005 mg·kg^(-1)、0.100 mg·kg^(-1)和0.500 mg·kg^(-1)3个加标水平下,52种农药残留的平均回收率为80.23%~99.43%,相对标准偏差为0.6%~6.3%。该方法具备操作简单、快速、准确以及灵敏度高等优点,适用于大批量六堡茶中多种农药残留量的快速测定。
A rapid method was developed for simultaneous determination of 52 pesticide residues in Liupao tea by solid phase extraction pretreatment and gas chromatography-tandem mass spectrometry.After crushing and sieving the sample,weighing 2.0 g of the sample,adding acetonitrile for ultrasonic extraction,concentrating the extraction solution to 2.0 mL,and then purifying it through a graphite carbon black amino composite solid-phase extraction column,the purified solution is analyzed by gas chromatography-tandem mass spectrometry,the standard curve was prepared by blank matrix liquid,and the peak area internal standard method was used for quantitative analysis.The results show that the correlation coefficients of 52 pesticide residue targets substances ranging from 0.005~0.500μg·mL-1were all greater than 0.995.The detection limits of the method was 0.002~0.030 mg·kg^(-1),the limits of quantification were 0.004~0.060 mg·kg^(-1).At three spiked levels of 0.005 mg·kg^(-1),0.100 mg·kg and 0.500 mg·kg^(-1),the average recoveries of 52 pesticide residues were 80.23%~99.43%and the relative standard deviations were 0.6%~6.3%.The method has the advantages of simple operation,fast,accurate and high sensitivity,and is suitable for the rapid determination of pesticide residues in large quantities of Liupao tea.
作者
文俊萍
蒋德莉
谭月媚
覃蓝
宋妤
WEN Junping;JIANG Deli;TAN Yuemei;QIN Lan;SONG Yu(Wuzhou Food and Drug Control Institute,Wuzhou 543000,China;Guangxi Key Laboratory of Liupao Tea Biology and Resource Utilization,Wuzhou 543000,China;Guangxi Engineering Research Center of Instant Liupao Tea,Wuzhou 543000,China;Guangxi Liupao Tea Scientific and Technological Achievements Transformation Pilot Research Base,Wuzhou 543000,China;Wuzhou Tianyu Tea Industry Co.,Ltd.,Wuzhou 543000,China)
出处
《食品安全导刊》
2024年第2期108-112,116,共6页
China Food Safety Magazine
基金
广西速溶六堡茶工程技术研究中心建设(厅市会商)(桂科AD20297077)。
