Disposable diapers are widely used in the US and many other areas in the world; therefore, they are ideal media for urine collection for measurement of young children's exposure to pesticides. However, disposable diapers normally contain polyacrylate polymers that make the extraction and analysis of urine very difficult. The objectives of this paper were to evaluate whether disposable diapers that contain polyacrylate granules can be extracted using salt solutions, and whether they can be used for the collection and quantitative measurements of selected urinary pyrethroid pesticide metabolites and creatinine. The storage stability of the metabolites and creatinine in a wet diaper at body temperature and at refrigeration temperature was also evaluated. Salt solutions including calcium chloride dihydrate, magnesium sulfate, ammonium acetate, and sodium chloride solutions were tested for efficiency of polymer shrinkage. Pyrethroid metabolites 3-(2,2-dichlorovinyl)-2,2-dimethyl-(1-cyclopropane) carboxylic acid (DCCA), 3-(2,2-dibromovinyl)-2,2,dimethyl-(1-cyclopropane) carboxylic acid (DBCA) and 3-phenoxybenzoic acid (3-PBA) were analyzed using LC/MS/MS and evaluated for recoveries in the urine released from the diapers. The study found calcium chloride dihydate to be satisfactory in releasing urine and metabolites from the polymers. The percent recoveries for the three tested pyrethroid metabolites were mostly in the range of 65-130. The percent recoveries for creatinine were in the range of 71-133. The detection limit for each of the three metabolites was 0.1 microg/l. The pyrethroid metabolites and creatinine were stable on the diaper for at least 72 h. We concluded from this study that calcium chloride dihydrate can successfully release urine and metabolites from polyacrylate-containing diapers, and the method is promising for studies of pyrethroid metabolites.