Determination of Nineteen Chlorophenols in Leather Products by Water Vapor Distillation-GC-MS

To determine content of chlorophenols in leather products, 1.000 g of samples was taken and added into 20 mL of 1 mol·L^-1 sulfuric acid solution and the chlorophenols in sample were extracted by water vapor distillation. Distillate obtained was reacted with potassium carbonate, thus to have chlorophenols converted into chlorinated phenyl potassium salt. After acetylated by acetic anhydride, these accetates were separated by DB-5MS chromatographic column with programmed temperature, and then determined by MS under EI and SIM mode. An internal standard method was adopted for quantification. As shown by results, when the mass concentrition of 19 chlorophenols was in the range of 1-40 μg·L^-1, ratio of mass concentration of their acetylation products between chlorophenols and the internal standard substance was linear with their respective ratios of peak area, with detection limits (3s) in the range of 0.006-0.015 mg·kg^-1. The recovery was made on blank leather products by standard addition method at 3 concentration levels, giving recoveries ranged from 85.7% to 105%. Values of RSDs (n=6) were found in the range of 2.3%-8.0%. The prescribed method was used for determination of 20 leather products, 3,5-DiCP, 2,4,6-TriCP, 2,3,4,6-TeCP and PCP were detected in 5 samples, with detection values in the range of 0.20-1.11 mg·kg^-1 and 5 detected values over the limit value (0.5 mg·kg^-1) given by GB/T 18885-2009.