色谱

色谱 ›› 2014, Vol. 32 ›› Issue (10): 1131-1137.DOI: 10.3724/SP.J.1123.2014.07028

• 研究论文 • 上一篇    下一篇

磁固相萃取-气相色谱-火焰光度检测联用测定果汁中的有机磷农药

黄倩, 何蔓, 陈贝贝, 胡斌   

  1. 武汉大学化学与分子科学学院, 生物医学分析化学教育部重点实验室, 湖北 武汉 430072
  • 收稿日期:2014-07-18 出版日期:2014-10-08 发布日期:2014-09-29
  • 通讯作者: 胡斌，E-mail：binhu@whu.edu.cn
  • 基金资助:

    国家自然科学基金项目（20975076）.

Magnetic solid phase extraction combined with gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in juice samples

HUANG Qian, HE Man, CHEN Beibei, HU Bin   

  1. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • Received:2014-07-18 Online:2014-10-08 Published:2014-09-29

PDF

320

被引次数

18

摘要：

制备了苯乙烯（St）和甲基丙烯酸（MAA）共聚物改性的磁性微球Fe3O4@P（St-co-MAA），并将其作为磁固相萃取吸附剂，建立了磁固相萃取（MSPE）-气相色谱（GC）-火焰光度检测（FPD）联用分析有机磷农药（OPPs）残留的新方法。以5种有机磷农药（二嗪农、甲基毒死蜱、杀螟硫磷、毒死蜱和喹硫磷）为目标分析物，考察并优化了吸附和解吸条件，确定了最佳实验条件。在最优的实验条件下，方法对5种OPPs的检出限（S/N=3）为0.013~0.305 μg/L，方法的相对标准偏差（RSD，n=7）为3.1%~8.8%，富集倍数为406~951，线性范围达3个数量级。将该方法应用于新鲜番茄汁、草莓汁样品中的OPPs残留分析，加标回收率为85.4%~118.9%。该方法具有检出限低、分析速度快、富集倍数高等优点，为有机磷农药的残留分析提供了新的技术平台。

关键词: 磁固相萃取, 果汁, 气相色谱-火焰光度检测, 有机磷农药

Abstract:

A novel method for the determination of organophosphorous pesticides (OPPs) in fresh juice samples was developed. Fe3O4@P(St-co-MAA) magnetic microparticles were synthesized and modified with styrene (St) and methacrylic acid (MAA) by coating St and MAA on magnetic particles and characterized by a series of techniques. The results indicated that Fe3O4 magnetic nanoparticles (MNPs) have been successfully modified with St and MAA. Based on the prepared Fe3O4@P(St-co-MAA) magnetic microparticles, a novel method of magnetic solid phase extraction (MSPE)-gas chromatography (GC)-flame photometric detection (FPD) was developed for the determination of OPPs. The extraction/desorption conditions of MSPE were optimized, and the analytical performance was evaluated under the optimal conditions. The limits of detection (LODs, S/N=3) for target OPPs were in the range of 0.013-0.305 μg/L with the RSDs (n=7) ranging from 3.1% to 8.8%. The enrichment factors varied from 406 to 951. The linear ranges were over three orders of magnitudes (R2>0.99) and the reproducibilities were 7.4%-14.5% (n=5). Finally, the proposed MSPE-GC-FPD method was successfully applied to the analysis of the five OPPs in fresh tomato and strawberry juice samples, with the recoveries of target OPPs in the range of 85.4%-118.9% for the spiked samples. The proposed MSPE-GC-FPD method is featured with low cost, fast separation and high enrichment factor.

Key words: gas chromatography-flame photometric detection (GC-FPD), juices, magnetic solid phase extraction (MSPE), organophosphorus pesticides (OPPs)

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