摘要
建立了固相微萃取-气相色谱-串联质谱法测定水生蔬菜中35种多氯联苯的方法。采用100μm聚二甲基硅氧烷萃取纤维,在萃取温度60℃、转动速度250 r/min的条件下萃取30 min,经气相色谱进样口280℃解吸6 min后,采用气相色谱-串联质谱法在时间选择反应监测模式下进行测定,外标法定量。结果表明,35种目标物在10~500μg/L内呈良好线性,线性相关系数均大于0.999,方法检出限为0.55~17.22 ng/kg;在0.01 mg/kg加标水平的平均回收率为72.3%~117.3%,相对标准偏差为1.2%~11.2%。该方法简便、快速、灵敏、准确,适用于水生蔬菜中多种多氯联苯残留量的快速测定。
A solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry method was developed for the determination of 35 polychlorinated biphenyls in aquatic vegetables. Samples were extracted with 100 μm polydimethylsiloxane at 60 ℃ for 30 min,and stirring at 250 r/min. After desorbed 6 min at 280 ℃ in gas chromatograph,sample extracts were injected and analyzed by GC-MS/MS at time selective reaction monitoring mode,and quantified by external standard method. The results showed that 35 target analysts displayed good linear relationships over concentration range of 10-500 μg/L,and correlation coefficients above 0. 999. The limits of detection were 0. 55-17. 22 ng/kg. The average recoveries of 35 compounds at two spiked levels of 0. 01 mg/kg ranged from 72. 3% to 117. 3%,with relative standard deviations of 1. 2% to 11. 2%. The advantages of simplicity,rapidness,sensitiveness and accuracy of the method was suitable for rapid detection of PCBs residues in aquatic vegetables.
作者
谢思思
卢俊文
李蓉
张朋杰
容裕棠
陈丽斯
XIE Si-si;LU Jun-wen;LI Rong;ZHANG Peng-jie;RONG Yu-tang;CHEN Li-si(Zhongshan Entry-Exit Inspection and Quarantine Bureau,Zhongshan 528400,Chin)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2018年第5期249-255,共7页
Food and Fermentation Industries
基金
广东省省级科技计划项目(2015A050502010
2014A040401011)
中山市科技计划项目(2016B2168)
关键词
固相微萃取
气相色谱-串联质谱
多氯联苯
水生蔬菜
solid-phase microextraction
gas chromatography-tandem mass spectrometry
polychlorinated biphenyls
aquatic vegetables
