乙腈-无机盐-水双水相体系萃取-气相色谱法检测鱼肉中拟除虫菊酯

doi:10.6023/A1106301

化学学报 ›› 2012, Vol. 0 ›› Issue (04): 485-491.DOI: 10.6023/A1106301 上一篇下一篇

研究论文

乙腈-无机盐-水双水相体系萃取-气相色谱法检测鱼肉中拟除虫菊酯

贾风燕, 王文文, 刘振波, 殷军港, 刘永明

烟台大学化学生物理工学院烟台 264005

投稿日期:2011-06-30 修回日期:2011-10-13 发布日期:2011-10-31
通讯作者: 刘永明
基金资助:
山东省科技攻关(No. 2009GG10009053)资助项目.

Extraction and Detection of Pyrethroids Pesticides in Fish Using Acetonitrile-Salt-H₂O System Coupled with Gas Chromatography

Jia Fengyan, Wang Wenwen, Liu Zhenbo, Yin Jungang, Liu Yongming

School of Chemical and Biological Science and Engineering, Yantai University, Yantai 264005

Received:2011-06-30 Revised:2011-10-13 Published:2011-10-31
Supported by:
Supported by the Project of Science and Technology of Shangdong Province (No. 2009GG10009053).

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摘要/Abstract

以乙腈-无机盐-水双水相体系, 建立了一种环保、高效的用于气相色谱法检测鱼肉样品中拟除虫菊酯的样品前处理方法. 实验利用荧光猝灭法与气相色谱法研究了拟除虫菊酯药物在以蛋白质为主要基质的水产品中的存在状态, 考察了双水相的形成条件, 并探讨了蛋白质对双水相萃取率的影响. 结果表明, 拟除虫菊酯药物通过疏水作用力与蛋白质牢固结合. 以体积分数为80%的乙腈水溶液作为萃取液可以引起水产品中的蛋白质基质缓慢而彻底地变性, 从而充分释放与蛋白质结合的药物, 实现拟除虫菊酯的均相高效萃取. 80%的乙腈水溶液具有较强的化学极性, 因而在双水相系统上相中与药物残留共同萃入的脂溶性杂质较少, 萃取液净化步骤大大简化. 在双水相上相中加入无水MgSO₄, PSA 去除水分与杂质后, 直接进样进行气相色谱检测. 该方法用于鱼肉样品中六种拟除虫菊酯的萃取检测, 回收率为 81.1%～96.4%, 检出限为8～14 ng·mL^-1.

关键词: 拟除虫菊酯, 双水相体系, 蛋白质, 乙腈, 气相色谱

Based on the acetonitrile-salt-H₂O aquatic two phase system, an effective sample pretreatment method was developed for the analysis of pyrethroids pesticides residues in fish by gas chromatography (GC). The fluorescence quenching method and GC were applied to study the form of pyrethroids pesticides in protein matrix of aquatic products. The influence factors on formation of acetonitrile-salt-H₂O system were discussed in depth. Meanwhile, the influence of the protein on extraction of pyrethroids pesticides from fish was detailedly investigated. The results showed that pyrethroids strongly bound with BSA by the hydrophobic interaction. In the φ(acetonitrile) 80%, a slow but full protein denaturation takes place, which causes the unfolding of protein and the release of pyrethroids. Then the drug residues was extracted into upper phase with high extraction efficiencies. Furthermore, the polarity of φ(acetonitrile) 80% is greater than φ (acetonitrile) 100%, the fat-soluble impurities are extracted less in φ(acetonitrile) 80% aqueous solution than that of in φ(acetonitrile) 100%. Therefore the purification steps were greatly simplified. The anhydrous magnesium sulfate (MgSO₄) and primary secondary amine (PSA) were added in upper phase to eliminate the moisture and other impurities. Then, the pyrethroids pesticides in extract (upper phase) was directly analyzed by GC. This method has been applied to the determination of pyrethroids pesticides residues in fish. The detection limits were in the range of 8～14 ng/mL, and the spiked recovery of fish were 81.1%～96.4%.

Key words: pyrethroids pesticides, aqueous two-phase system, protein, acetonitrile, gas chromatography

引用此文

贾风燕, 王文文, 刘振波, 殷军港, 刘永明. 乙腈-无机盐-水双水相体系萃取-气相色谱法检测鱼肉中拟除虫菊酯[J]. 化学学报, 2012, 0(04): 485-491.

Jia Fengyan, Wang Wenwen, Liu Zhenbo, Yin Jungang, Liu Yongming. Extraction and Detection of Pyrethroids Pesticides in Fish Using Acetonitrile-Salt-H₂O System Coupled with Gas Chromatography[J]. Acta Chimica Sinica, 2012, 0(04): 485-491.

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乙腈-无机盐-水双水相体系萃取-气相色谱法检测鱼肉中拟除虫菊酯

Extraction and Detection of Pyrethroids Pesticides in Fish Using Acetonitrile-Salt-H₂O System Coupled with Gas Chromatography

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乙腈-无机盐-水双水相体系萃取-气相色谱法检测鱼肉中拟除虫菊酯

Extraction and Detection of Pyrethroids Pesticides in Fish Using Acetonitrile-Salt-H2O System Coupled with Gas Chromatography

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Extraction and Detection of Pyrethroids Pesticides in Fish Using Acetonitrile-Salt-H₂O System Coupled with Gas Chromatography