摘要
建立同时测定蛋及蛋制品中六六六、滴滴涕和指示性多氯联苯残留量的双重净化-气相色谱法。样品经乙腈提取,浓硫酸和焙烧型水滑石双重净化后采用气相色谱分析和外标法定量。结果表明：与传统的磺化法相比,采用浓硫酸和焙烧型水滑石双重净化的效果更好,干扰物质少,且目标物提取更充分。在10～200 μg/L的添加水平内4种六六六、2种滴滴涕和7种指示性多氯联苯的线性关系良好,相关系数均大于0.999。方法的检出限（RSN=3）范围为1.12～3.89 μg/kg,定量限（RSN=10）范围为3.73～12.97 μg/kg。添加10、20、100μg/kg3 个水平的4种六六六、2种滴滴涕和7种指示性多氯联苯于鸡蛋液、咸蛋及皮蛋空白样品中,加标回收率范围为78.04%～105.05%,相对标准偏差范围为1.28%～7.55%。该方法操作简便快速、准确、灵敏,适用于蛋及蛋制品中六六六、滴滴涕和指示性多氯联苯残留量的快速测定。
A double depuration-gas chromatography（DDGC） method was developed for the simultaneous determination of residues of hexachlorocyclohexanes（BHCs）,dichlorodiphenyltrichloroethanes（DDTs） and indicator polychlorinated biphenyls（PCBs） in eggs and egg products.Samples were extracted with acetonitrile followed by double purification with concentrated sulfuric acid and calcined hydrotalcite.Then the analytes were analyzed by GC and quantified with an external standard method.Results showed that compared with the traditional sulfonation method,more thorough extraction and higher purification efficiency of the target analytes with less interferences were achieved by double-purification with concentrated sulfuric acid and calcined hydrotalcite.Good linearities were obtained for four BHCs,two DDTs,and seven PCBs with correlation coefficients greater than 0.999 in the range of 10–200 μg/L.The limits of detection（LODs）（RSN = 3） and limits of quantitation（LOQs）（RSN =10） of the GC method were 1.12–3.89 and 3.73–12.97 μg/kg,respectively.The recoveries of these analytes from liquid egg,preserved eggs and salted eggs ranged from 78.04% to 105.05%,with relative standard deviation（RSD） ranging from 1.28% to 7.55% at three spiked levels of 10,20,and 100 μg/kg.The method was simple,rapid,accurate and sensitive,and it was suitable for rapid detection of PCBs,BHCs and DDTs residues in eggs and egg products.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2016年第24期222-227,共6页
Food Science
基金
国家质检总局科技项目(2015IK033)
国家自然科学基金青年科学基金项目(31401597)
福建出入境检验检疫局科技项目(FK2013-19)
福建省科技计划项目(2016Y0085)
福建省高水平大学建设项目(612014043)
2015年中青年教师教育科研项目杰出人才计划项目
关键词
蛋
蛋制品
六六六
滴滴涕
指示性多氯联苯
气相色谱法
eggs
egg products
hexachlorocyclohexanes（BHCs）
dichlorodiphenyltrichloroethanes（DDTs）
indicator polychlorinated biphenyls（PCBs）
gas chromatography（GC）
