title: Supercritical-fluid extraction of synthetic pyrethroids from wool.
abstract: A stepwise approach was used to develop a supercritical fluid extraction (SFE) method for analysis of synthetic pyrethroids (SPs) on a wool matrix, commencing with a simple inert matrix to examine the solubility of the pyrethroids in the extraction fluid CO(2) and then extended to the real wool matrix. Chemometric approaches were used to determine the SFE optimum conditions. It was found that pyrethroids were readily extractable from an inert matrix over a wide range of pressure (170-350 atm) and at low temperature (<90 degrees C). Subambient hexane efficiently trapped the compounds from the depressurised fluid. Excessively high pressure and temperature resulted in poor trapping, isomerisation and possibly degradation of some components. With spiked wool samples method modifications focused on reducing the coextraction of grease, a bulk matrix component of raw wool. By using alumina (containing 8% moisture) and operating the extraction at 50 degrees C, 200 atm for 60 min, sufficiently clean extracts of pyrethroids suitable for gas chromatography-electron-capture detection analysis were obtained. The recoveries of all SPs were satisfactory (78-101%) over the range of 0.5-5 microg/g levels of these compounds. The precision of the entire analysis procedure was comparable to the conventional Soxhlet extraction method. Detection limits of some commonly used SPs for sheep treatment were also evaluated. Comparable results relative to those achieved by solvent extraction for incurred wool samples were obtained with a recovery of 81-85%. The results, however, suffered high uncertainties (R.S.D. approximately 19-24%) due to the small amount of wool sample taken in each extraction and the suspected inhomogeneity of the wool. Different persistences of cypermethrin isomers in wool were observed.
authors.affiliation: Chromatography and Molecular Separations Group, Department of Applied Chemistry, Royal Melbourne Institute of Technology, GPO Box 2476V, Victoria 3001, Melbourne, Australia.
authors.forename: A M
authors.initials: AM
authors.lastname: Nguyen
authors.forename: P J
authors.initials: PJ
authors.lastname: Marriott
authors.forename: J
authors.initials: J
authors.lastname: Hughes
mesh_terms: D000537:Aluminum Oxide / Q000737:chemistry; D000818:Animals; D002245:Carbon Dioxide / Q000737:chemistry; D002845:Chromatography / Q000379:methods*; D002849:Chromatography, Gas / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry; D015233:Models, Statistical; D009570:Nitriles; D010575:Pesticides / Q000032:analysis*; D011312:Pressure; D011722:Pyrethrins / Q000032:analysis; D013696:Temperature; D013997:Time Factors; D014935:Wool / Q000737:chemistry*
chemical_list: D009570:Nitriles; D010575:Pesticides; D011722:Pyrethrins; D002245:Carbon Dioxide; C017180:decamethrin; D000537:Aluminum Oxide; C052570:cyfluthrin; C009424:tetramethrin