Dynamic headspace time-extended helix liquid-phase microextraction.
Liquid-phase microextraction (LPME) has been proved to be a fast, inexpensive and effective sample pre-treatment technique for the analyses of pesticides and many other compounds. In this investigation, a new headspace microextraction technique, dynamic headspace time-extended helix liquid-phase microextraction (DHS-TEH-LPME), is presented. In this work, use of a solvent cooling system, permits the temperature of the extraction solvent to be lowered. Lowering the temperature of the extraction solvent not only reduces solvent loss but also extends the feasible extraction time, thereby improving extraction efficiency. Use of a larger volume of the solvent not only extends the feasible extraction time but also, after extraction, leaves a larger volume to be directly injected into the gas chromatography (GC) to increase extraction efficiency and instrument signal. The DHS-TEH-LPME technique was used to extract six organochlorine pesticides (OCPs) from 110ml water samples that had been spiked with the analytes at ng/l levels, and stirred for 60min. The proposed method attained enrichments up to 2121 fold. The effects of extraction solvent identity, sample agitation, extraction time, extraction temperature, and salt concentration on extraction performance were also investigated. The method detection limits (MDLs) varied from 0.2 to 25ng/l. The calibration curves were linear for at least 2 orders of magnitude with R(2)>==0.996. Relative recoveries in river water were more than 86%.
Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan.
Shih-Pin
SP
Huang
Pai-Shan
PS
Chen
Shang-Da
SD
Huang
D005591:Chemical Fractionation / Q000379:methods*; D006843:Hydrocarbons, Chlorinated / Q000737:chemistry*; D010575:Pesticides / Q000737:chemistry*; D013696:Temperature
D006843:Hydrocarbons, Chlorinated; D010575:Pesticides