分散固相萃取-气质联用法测定果汁中邻苯基苯酚残留量  

Determination of o-phenylphenol residues in fruit juice by dispersive solid phase extraction-gas chromatography-mass spectrometry

作　　者：丁立平 DING Liping(Rongcheng Customs and Excise Integrated Technical Service Centre,Fuqing 350300,China)

机构地区：[1]榕城海关综合技术服务中心,福清350300

出　　处：《分析试验室》2022年第8期915-919,共5页Chinese Journal of Analysis Laboratory

基　　金：福建省引导性科技计划项目(2018Y0085,2016Y0085);海关总署科技计划项目(2017IK189);福州市科技计划项目(2020-S-35);福州海关科技项目(FK2020-01)资助

摘　　要：以新型材料对甲基苯磺酸根-镁铝型水滑石为分散固相萃取吸附剂,建立了分散固相萃取-气质联用法测定果汁中邻苯基苯酚残留量。果汁以去离子水稀释后,经吸附剂以分散固相萃取方式吸附、离心、酸溶解吸附剂、乙酸丁酯萃取后采用气质联用法对邻苯基苯酚测定,以基质匹配校正曲线外标法定量。结果表明:果汁在1~10μg/L添加水平范围内邻苯基苯酚的平均回收率为92.5%~96.8%,相对标准偏差(RSD)为2.2%~4.9%;方法检出限(LOD)为2.05μg/L,定量限(LOQ)为6.85μg/L。本方法适合果汁中邻苯基苯酚残留量的检测。A new material named as p-toluenesulfonate-Mg-Al hydrotalcite was used as a dispersive solid-phase extraction adsorbent for the determination of o-phenylphenol residues in fruit juice by gas chromatography-mass spectrometry.The fruit juice was diluted with deionized water,adsorbed by adsorbent using dispersive solid phase extraction.Then the adsorbent was centrifuged and dissolved with acid.The o-phenylphenol residues were extracted with butyl acetate,determined by gas chromatography-mass spectrometry and quantified by matrix matching correction curve in external standard method.The average fortified recoveries of o-phenylphenol in fruit juice were found in the range of 92.5%-96.8%at three fortified levels from 1 to 10μg/L,with the relative standard deviations of 2.2%-4.9%,while the limits of detection and quantification were 2.05μg/L and 6.85μg/L,respectively.The developed method is suitable for the detection of o-phenylphenol residues in fruit juice.

关 键 词：果汁 邻苯基苯酚 对甲基苯磺酸根-镁铝型水滑石 气质联用法 分散固相萃取 

分 类 号：O657.63[理学—分析化学]