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  • Title: Determination of organochlorine pesticides in water using solvent cooling assisted dynamic hollow-fiber-supported headspace liquid-phase microextraction.
    Author: Huang SP, Huang SD.
    Journal: J Chromatogr A; 2007 Dec 28; 1176(1-2):19-25. PubMed ID: 18001752.
    Abstract:
    The organic solvent film formed within a hollow fiber was used as an extraction interface in the headspace liquid-phase microextraction (HS-LPME) of organochlorine pesticides. Some common organic solvents with different vapor pressures (9.33-12,918.9 Pa) were studied as extractants. The results indicated that even the solvent with the highest vapor pressure (cyclohexane) can be used to carry out the extraction successfully. However, those compounds (analytes) with low vapor pressures could not be extracted successfully. In general, the large surface area of the hollow fiber can hasten the extraction speed, but it can increase the risk of solvent loss. Lowering the temperature of the extraction solvent could not only reduce solvent loss (by lowering its vapor pressure) but also extend the feasible extraction time to improve extraction efficiency. In this work, a solvent cooling assisted dynamic hollow-fiber-supported headspace liquid-phase microextraction (SC-DHF-HS-LPME) approach was developed. By lowering the temperature of the solvent, the evaporation can be decreased, the extraction time can be lengthened, and, on the contrary, the equilibrium constant between headspace phase and extraction solvent can be increased. In dynamic LPME, the extracting solvent is held within a hollow fiber, affixed to a syringe needle and placed in the headspace of the sample container. The extracting solvent within the fiber is moved to-and-fro by using a programmable syringe pump. The movement facilitates mass transfer of analyte(s) from the sample to the solvent. Analysis of the extract was carried out by gas chromatography-mass spectrometry (GC-MS). The effects of identity of extraction solvent, extraction temperature, sample agitation, extraction time, and salt concentration on extraction performance were also investigated. Good enrichments were achieved (65-211-fold) with this method. Good repeatabilities of extraction were obtained, with RSD values below 15.2%. Detection limits were 0.209 microg/l or lower.
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