摘要
建立了全自动凝胶净化-气相色谱质谱联用法同时测定水果中邻苯基苯酚、增效醚残留量的方法,即脐橙、梨、菠萝等3种水果样品经粉碎后,加入丙酮+二甲苯(体积比2∶1)超声波提取16 min,经全自动凝胶色谱系统(GPC)净化、浓缩、定容后,用气相色谱质谱联用仪测定邻苯基苯酚、增效醚残留量,并以环氧七氯为内标物进行定量。结果表明,该方法的相关系数均达到0.999以上,定量下限均小于0.02 mg/kg;添加25、50、100μg/kg 3个水平的邻苯基苯酚和增效醚于脐橙、梨、菠萝空白样品中,加标回收率范围为80.2%～107.8%,相对标准偏差范围为0.9%～2.9%。该测定方法操作简便、快速、准确、灵敏、重现性好,适用于水果中邻苯基苯酚和增效醚残留量的快速分析测定。
A method for simultaneous determination of o-phenylphenol and piperonyl butoxide in fruits by automatic gel purification-gas chromatography-mass spectrometry was developed.Samples of three kinds of fruits,such as navel orange,pear and pineapple,were crushed and added with acetone+xylene(2+1)for ultrasonic extraction of 16min.After being purified,concentrated and fixed by automatic gel chromatography(GPC),the residual amount of o-phenylphenol and piperonyl butoxide was determined by gas chromatography-mass spectrometry ( GC-MS ),and heptachlor epoxide was used as internal standard for quantitative analysis.The results showed that the correlation coefficients of the method were all above 0.999, and the lower limit of quantification was less than 0.02 mg/kg.25,50 and 100 μg/kg of o-phenylphenol and piperonyl butoxide were added to the blank samples of orange,pear and pineapple,the recoveries rate were 80.2%-107.8%,and the relative standard deviation was 0.9%-2.9%.The method is simple,rapid,accurate,sensitive and reproducible,so it is suitable for the rapid determination of o-phenylphenol and piperonyl butoxide residues in fruits.
作者
李世艳
鲁佳
郭庆
LI Shi-yan;LU Jia;GUO Qing(Bengbu Institute of Product Quality Supervision and Inspection Research,Bengbu Anhui 233040)
出处
《现代农业科技》
2019年第5期103-105,共3页
Modern Agricultural Science and Technology
