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用于环境水样中有机磷农药定量分析的固相微萃取

Solid-phase microextraction for quantitative analysis of organophosphorus pesticides in environmental water samples.

作者信息

Beltran J, Lopez F J, Cepria O, Hernandez F

机构信息

Experimental Sciences Department, University Jaume I, Castellon, Spain.

出版信息

J Chromatogr A. 1998 May 29;808(1-2):257-63. doi: 10.1016/s0021-9673(98)00138-1.

DOI:10.1016/s0021-9673(98)00138-1
PMID:9678959
Abstract

Solid-phase microextraction (SPME) is a relatively new technique that appears as a convenient and efficient extraction method in contrast with more complex techniques used for pesticide residue analysis based on liquid-liquid and solid-phase extraction. This extraction procedure involves the absorption of analytes into a polymeric film coated onto a fine silica fiber directly dipped in the aqueous sample. An SPME procedure for the determination of 12 organophosphorus pesticides in clean environmental water samples at low ng/ml concentration level has been developed by optimising variables involved in extraction and desorption. The absorption equilibrium has been estimated by mathematical treatment of the process using an expression that describes experimental absorption time profiles. The method was evaluated according to the reproducibility, linearity range and limits of detection using two different fiber coatings: 100 microm polydimethylsiloxane and 85 microm polyacrylate. The limits of detection obtained using nitrogen-phosphorus detection ranged between 0.01 and 0.2 ng/ml with relative standard deviations lower than 15% at the 1 ng/ml level. The method showed good linearity between 0.1 and 10 ng/ml with regression coefficients ranging between 0.97 and 0.999. Determination of organophosphorus pesticides in water samples in concentration below 0.1 ng/ml can be easily carried out with this fast, economic and solvent-free SPME procedure.

摘要

固相微萃取(SPME)是一种相对较新的技术,与基于液-液萃取和固相萃取的更复杂的农药残留分析技术相比,它是一种方便高效的萃取方法。这种萃取过程涉及将分析物吸收到直接浸入水样中的涂覆在细石英纤维上的聚合物薄膜中。通过优化萃取和解吸过程中的变量,开发了一种用于测定清洁环境水样中低纳克/毫升浓度水平的12种有机磷农药的固相微萃取方法。通过使用描述实验吸收时间曲线的表达式对该过程进行数学处理来估计吸收平衡。使用两种不同的纤维涂层:100微米聚二甲基硅氧烷和85微米聚丙烯酸酯,根据重现性、线性范围和检测限对该方法进行了评估。使用氮磷检测获得的检测限在0.01至0.2纳克/毫升之间,在1纳克/毫升水平下相对标准偏差低于15%。该方法在0.1至10纳克/毫升之间显示出良好的线性,回归系数在0.97至0.999之间。使用这种快速、经济且无溶剂的固相微萃取方法可以轻松测定浓度低于0.1纳克/毫升的水样中的有机磷农药。

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