College of Science, China Agricultural University, Beijing 100193, China.
J Chromatogr A. 2013 Oct 11;1311:41-7. doi: 10.1016/j.chroma.2013.08.080. Epub 2013 Aug 27.
A novel and simple air-assisted liquid-liquid microextraction (AALLME) is introduced to analyze the organophosphorus pesticide (OPP) residues in fruit juice samples, using the gas chromatography-flame photometric detection (GC-FPD). In this method, fine extraction solvent drops are rapidly formed and dispersed into the aqueous samples, by using a syringe to withdraw and push-out the mixture of aqueous sample solution and extraction solvent several times. The parameters affecting the extraction efficiency were investigated including the type and volume of the extraction solvent, salt addition, extraction times, and pH. Under optimized conditions, the method showed good linearities with the correlation coefficients (γ) higher than 0.9988, and the sensitivity with the limits of detection (LODs) between 0.02μgL(-1) and 0.6μgL(-1). The method was applied to determine the OPP residues in juice samples and the recoveries were ranged from 79% to 113% with relative standard deviations (RSDs) of 0.4-9.9%. The feasibility of the method in real samples was proved.
介绍了一种新颖而简单的气助液-液微萃取（AALLME）方法，用于分析果汁样品中的有机磷农药（OPP）残留，采用气相色谱-火焰光度检测（GC-FPD）。在该方法中，通过注射器多次抽取和推出水相样品溶液和萃取溶剂的混合物，迅速形成并分散精细的萃取溶剂液滴到水相中。研究了影响萃取效率的参数，包括萃取溶剂的类型和体积、加盐、萃取次数和 pH 值。在优化条件下，该方法具有良好的线性关系，相关系数（γ）高于 0.9988，灵敏度的检出限（LODs）在 0.02μgL(-1)和 0.6μgL(-1)之间。该方法用于测定果汁样品中的 OPP 残留，回收率在 79%至 113%之间，相对标准偏差（RSD）为 0.4-9.9%。该方法在实际样品中的可行性得到了验证。
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