Journal of chromatography. A 2015-01-16

Fast agitated directly suspended droplet microextraction technique for the rapid analysis of eighteen organophosphorus pesticides in human blood.

Rupender Kumari, Devendra K Patel, Smita Panchal, Rakesh R Jha, G N V Satyanarayana, Ankita Asati, Nasreen G Ansari, Manoj K Pathak, C Kesavachandran, Ramesh C Murthy

文献索引：J. Chromatogr. A. 1377 , 27-34, (2015)

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摘要

A new sample preparation technique named as fast agitated directly suspended droplet microextraction (FA-DSDME) was proposed as an improved version of directly suspended droplet microextraction (DSDME) for the extraction and pre-concentration of wide-range organophosphorus pesticides (OPPs) from human blood prior to liquid chromatography tandem mass spectrometric (LC-MS/MS) analysis. In this method, instead of protecting the unwanted rupturing of extraction droplet (organic solvent), it was deliberately splintered into fine droplets by providing automated high-speed agitation to the biphasic extraction system (extraction solvent and sample solution). Fine organic droplets were then recollected into one, not by using a centrifuge machine but just by giving a very slow stirring to the bottom of the extraction system. The present method has surmounted the problem of prolonged extraction time associated with old DSDME. Under optimum extraction conditions, the method showed good sensitivity with low detection limits ranging from 0.0009 to 0.122μgL(-1). Mean recoveries were achieved in the range of 86-109% at three levels of spiking concentration (low, middle and high) from linearity range of individual analyte. Intra-day and inter-day precisions were ≤4.68 and ≤9.57 (%RSD) respectively. Enrichment factor (EF) for each analyte varied from 30 to 132 which prove the ability of this technique to pre-concentrate the extracted analytes up to a good extent. The sample matrices have shown an insignificant influence on method's sensitivity. The proposed method may find immense use in epidemiological, toxicological, regulatory and forensic laboratories. Copyright © 2014 Elsevier B.V. All rights reserved.