4.7 Article

The development and optimization of a modified single-drop microextraction method for organochlorine pesticides determination by gas chromatography-tandem mass spectrometry

期刊

MICROCHIMICA ACTA
卷 178, 期 1-2, 页码 195-202

出版社

SPRINGER WIEN
DOI: 10.1007/s00604-012-0810-9

关键词

Organochlorine pesticides; SDME; GC-MS/MS

资金

  1. FCT (Fundacao para a Ciencia e a Tecnologia) [BD/47200/2008, PEst-C/EQB/LA0006/2011]

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We have developed a new method for single-drop microextraction (SDME) for the preconcentration of organochlorine pesticides (OCP) from complex matrices. It is based on the use of a silicone ring at the tip of the syringe. A 5 mu L drop of n-hexane is applied to an aqueous extract containing the OCP and found to be adequate to preconcentrate the OCPs prior to analysis by GC in combination with tandem mass spectrometry. Fourteen OCP were determined using this technique in combination with programmable temperature vaporization. It is shown to have many advantages over traditional split/splitless injection. The effects of kind of organic solvent, exposure time, agitation and organic drop volume were optimized. Relative recoveries range from 59 to 117 %, with repeatabilities of < 15 % (coefficient of variation) were achieved. The limits of detection range from 0.002 to 0.150 mu g kg(-1). The method was applied to the preconcentration of OCPs in fresh strawberry, strawberry jam, and soil.

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