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渔业研究 ›› 2018, Vol. 40 ›› Issue (1): 60-65.

• 论文与报告 • 上一篇    下一篇

同位素稀释-气相色谱-质谱法测定河蚌蚌肉中邻苯二甲酸酯类残留量

姑丽巴哈尔·艾合买提1,阿依古丽.塔西2   

  1. 1. 新疆维吾尔自治区分析测试研究院
    2.
  • 收稿日期:2017-11-16 修回日期:2017-12-05 出版日期:2018-02-26 发布日期:2018-03-05
  • 通讯作者: 姑丽巴哈尔·艾合买提

Determination of phthalate acid ester residues in the meat of freshwater mussel by gas chromatography-mass spectrometry

  1. 1. Xinjiang Uygur Autonomous Region Academy of Instrument Analysis
    2.
  • Received:2017-11-16 Revised:2017-12-05 Online:2018-02-26 Published:2018-03-05

摘要: 河蚌蚌肉样品采用乙酸乙酯溶剂提取,滤液经弗罗里硅土固相萃取柱净化后氮吹浓缩,正己烷定容,经气质联用仪进行检测,同位素内标法定量。实验结果表明:PAEs在0.10 ~2.00 mg/L之间具有良好的线性关系,相关系数r2均大于0.99,对样品进行高、中、低三个浓度的加标试验,各组分的平均回收率在73.1%~94.3%之间,相对标准偏差(RSD)值小于9.3%,检出限在1.2~3.9 μg/kg之间。该方法前处理简单,灵敏度和准确度高,可满足河蚌蚌肉中邻苯二甲酸酯类化合物的残留量检测要求。

关键词: 邻苯二甲酸酯(PAEs), 河蚌, 气质联用, PAEs, freshwater mussel meat, GC-MS

Abstract: The freshwater mussel samples were extracted with ethyl acetate solvent. Then the samples were purified by solid-phase extraction with Florisil column. After filtration, the filtrate was concentrated with nitrogen and concentrated with n-hexane. The content was determined by gas chromatography-mass spectrometry (GC-MS) with isotope internal standard method. The results showed that: PAEs had a good linear relationship between 0.10-2.00 mg/L, while the correlation coefficient r were all above 0.99. The average recoveries ranged from 73.1% to 94.3% with RSD that less than 9.3% by three level of spiked concentrations. The limit of detection were ranged from 1.2 to 3.9 μg/kg. The method had the advantages of simple pretreatment, high sensitivity and high accuracy, and can be satisfied in requirement of detecting phthalate residues in freshwater mussel meat.