气相色谱法测定咖啡生豆中硫丹及硫丹硫酸酯残留  

Determination of Endosulfan and Endosulfan Sulfate Residues in Coffee Beans by Gas Chromatography

作　　者：蒲泓君 邓洪燕 满红平 PU Hongjun;DENG Hongyan;MAN Hongping(Pu’er Comprehensive Technical Testing Center,Pu’er 665000,China;College of Tropical Crops,Yunnan Agricultural University,Pu’er 665000,China)

机构地区：[1]普洱市质量技术综合检测中心,云南普洱665000 [2]云南农业大学热带作物学院,云南普洱665000

出　　处：《食品安全导刊》2023年第12期102-105,共4页China Food Safety Magazine

摘　　要：建立气相色谱测定咖啡中α-硫丹、β-硫丹和硫丹硫酸酯残留的方法。咖啡粉末样品经过乙腈超声提取,离心后上清液依次经安捷伦增强型除脂分散净化管EMR-Lipd、1.6 g硫酸镁和0.4 g氯化钠和弗罗里硅小柱净化,50℃氮吹仪上浓缩至近干,加入1.00 mL正己烷复溶,用毛细管柱气相色谱分离测定。3种有机氯农药在0.01~0.50μg·mL^(-1)线性相关性良好,相关系数均大于0.995,检出限为0.0022~0.0044 mg·kg^(-1),测定下限为0.01~0.02 mg·kg^(-1)。在0.02~0.10 mg·kg^(-1)的加标水平下,3种农药的加标回收率为80.1%~94.1%,相对标准偏差为2.4%~9.1%。因此,该方法前处理对咖啡油脂的净化较佳,准确度和精密度满足实验室要求,可用于定性及定量检测咖啡中硫丹及其代谢物农药残留。A gas chromatography method for the determination ofα-endosulfan,β-endosulfan and endosulfan sulfate residues in coffee was established.The coffee powder samples were ultrasonic extracted by acetonitrile extraction.After centrifugation,the supernatant was purified by Agilent enhanced EMR-Lipd,1.6 g magnesium sulfate,0.4 g sodium chloride and Flori silicon column,concentrated to nearly dry on a nitrogen blower at 50℃,and 1.00 mL n-hexane was added for resolution.The capillary column was separated by gas chromatography,and the retention time and peak area were qualitatively determined by electron capture detector.The three organochlorine pesticides had good linear correlation in 0.01~0.50μg·mL-1,and the correlation coefficients were all greater than 0.995.The limit of detection was 0.0022~0.0044 mg·kg^(-1),and the limit of quantitation was 0.01~0.02 mg·kg^(-1).The recoveries ranged from 80.1%to 94.1%and the relative standard deviations ranged from 2.4%to 9.1%at 0.02~0.10 mg·kg^(-1).Therefore,the method can be used for qualitative and quantitative determination of endosulfan and its metabolites pesticide residues in coffee,and its accuracy and precision meet the laboratory requirements.

关 键 词：气相色谱法 硫丹及其代谢物 咖啡生豆 

分 类 号：TS273[轻工技术与工程—农产品加工及贮藏工程] O657.71[轻工技术与工程—食品科学与工程]