Development of an improved single-drop microextraction method and its application for the analysis of carbamate and organophosphorus pesticides in water samples

• Published in: Analyst (London) Vol. 137; no. 22; pp. 5339 - 5345
• Main Authors: Wang, Xiuhong, Cheng, Jing, Wang, Xiangfang, Wu, Min, Cheng, Min
• Format: Journal Article
• Language: English
• Published: Cambridge Royal Society of Chemistry 21.11.2012
• Subjects: Analytical chemistry; Carbamates - analysis; Carbamates - isolation & purification; Chemical Fractionation - instrumentation; Chemical Fractionation - methods; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid; Exact sciences and technology; Hydrogen-Ion Concentration; Organophosphorus Compounds - analysis; Organophosphorus Compounds - isolation & purification; Other chromatographic methods; Pesticides - analysis; Pesticides - isolation & purification; Salts - chemistry; Solvents - chemistry; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - isolation & purification; Water; Microanalysis; HPLC chromatography; Solvent extraction; Chemical enrichment; Improvement; Sample preparation; Efficiency; Detection limit; Standard deviation; Solvent; Trace analysis; Factor analysis; Stability; Device; Sample; Use; Pesticides; Method; Polymerase chain reaction; Repeatability; Microextraction; Parameter; Organophosphorus compounds; Detection; Application; Carbamate
• ISSN: 0003-2654; 1364-5528
• DOI: 10.1039/c2an35623f

An improved single-drop microextraction (SDME) method combined with high performance liquid chromatography has been developed for the detection of trace carbamate and organophosphorus pesticides in water samples. The most fascinating feature of the proposed method is the use of an oval-shaped polychloroprene rubber (PCR) tube to load the extraction solvent, which efficiently loads more solvent and improves the stability of extraction microdrop. Furthermore, this device provides a larger contact surface between the extraction solvent and the inner surface of the oval-shaped PCR tube than that between the extraction solvent and the tip of a microsyringe needle in the conventional SDME. It thereby avoids the problem of the drop floating upwards or dislodging from the tip of the microsyringe needle as observed in the traditional SDME. This method is significant for the great improvement it can offer in extraction efficiency. A series of extraction parameters were investigated systematically using carbamate and organophosphorus as the model analytes. Under the optimal conditions, the enrichment factors for analysis were between 117 and 177, and the limits of detection were 0.63 μg L −1 ( S / N = 3). The repeatability study was carried out by extracting the spiked water samples. Here the relative standard deviations varied between 4.0 and 5.8% ( n = 5). Additionally, the proposed method was successfully applied to the determination of pesticides in real water samples, and good recoveries were obtained from 79% to 112%. The proposed method was demonstrated to hold advantages of low cost, simplicity of operation, and successful application to in real water samples. In this method, a novel device was designed as a holder, which can load more solvent and improve the stability of extraction solvent microdrop.