Determination of Pentachlorophenol Residues in Textiles and Leather and Leather Products by Gas Chromatography/Mass Spectrometry
纺织品、皮革及其制品中五氯苯酚残留量的气相色谱-质谱法测定

A method for determination of pentachlorophenol residues in textiles and leather and leather products by gas chromatography/mass spectrometry was developed. The pentachlorophenol residues in samples was acidified with sulphuric acid solution (6 mol/L) and extracted with n-hexane. After the n-hexane layer was washed with sodium sulphate solution (20 g/L)until it was clear, determination was made by means of a gas chromatograph equipped with MSD, using external standard method. A DB-17 fused silica capillary column (30 m x 0.25 mm i.d.; 0.25 micron film thickness) was employed in the analysis, The column temperature program included a 2 min isothermal period at 50 degrees C, temperature increased at a rate of 30 degrees C/min to 220 degrees C, and hold for 1 min; temperature increased of at a rate 6 degrees C/min to 260 degrees C, and hold for 1 min. Mass spectra were obtained by electron impact at 70 eV and the determination was made by means of SIM mode, selected monitoring ion (m/z) was 264 amu. The detection limit was 0.02 mg/kg. The average recovery was from 86.7% to 93.1% and CV (n = 10) is from 4.1% to 5.9%. This method was already used to determine the mass concentration of pentachlorophenol residues in raw cotton, towel, shirt, leather gloves, leather watchguard. The method is simple, rapid and accurate.