高效液相色谱法同时测定纺织品中10种酚类化合物

Simultaneous Determination of Ten Phenols in Textiles by High Performance Liquid Chromatography

建立了高效液相色谱法同时测定纺织品中五氯苯酚、2,3,4,5-四氯苯酚、2,3,4,6-四氯苯酚、2,3,5,6-四氯苯酚、2,4,5-三氯苯酚、2,4,6-三氯苯酚、邻苯基苯酚、间羟基联苯、2-萘酚、对硝基苯酚10种酚类化合物的检测方法。纺织品中的酚类化合物经甲醇超声提取、浓缩后,以ZORBAX SB-C18柱(4.6 mm×150 mm,5μm)为分析柱,乙腈和0.01 mol/L磷酸溶液为流动相梯度洗脱,采用二极管阵列检测器,在220 nm和310 nm波长下进行高效液相色谱检测,紫外光谱库确证,外标法定量。10种酚类化合物在0.3～37 mg/L浓度范围内与其峰面积呈良好的线性关系,相关系数为0.999 1～0.999 5;以不低于3倍的信噪比计算10种酚类化合物的检出限(LOD)为0.003 0～0.041 1 mg/kg;定量下限(LOQ,S/N≥10)为0.010 0～0.1370 mg/kg。棉、麻、毛3种纺织品基质在3个不同加标水平的回收率为81%～105%,相对标准偏差(RSDs)为1.7%～8.5%。该方法能同时完成10种酚类化合物的确证和分析,可用于纺织品中酚类化合物残留的检测分析。

A high performance liquid chromatographic （HPLC） method was developed for the simultaneous extraction and determination of ten phenols, including pentachlorophenol, 2, 3, 4, 5-tetrachlorophenol, 2, 3, 4, 6-tetrachlorophenol, 2, 3, 5, 6-tetrachlorophenol, 2, 4, 5-trichlorophenol, 2, 4, 6-trichlorophenol, 2-phenylphenol, 3-phenylphenol, 2-naphthol and 4-nitrophenol in textiles. The samples were ultrasonically extracted with methanol. The separation and quantification of ten phenols were achieved on an ZORBAX SB - C_18 column（4. 6 mm x 150 mm, 5 Ixm ） with mobile phase of aeetonitrile -0. 01 mol/L phosphate and the diode array detector（DAD） at 220 nm and 310 nm. Lab-buih UV spectroscopy library and external standards were employed for the identification and quantification of target compounds. The result indicated that the calibration curves of ten phenols showed good linear relationships between peak areas and concentrations in the range of 0. 3 - 37 mg/L, with their correlation coefficients of 0. 999 1 -0. 999 5. The limits of detection（ LODs, S/ N≥3） of ten phenols were in the range of 0. 003 0 -0. 041 1 mg/kg, and the limits of quantitation （LOQs, S/N≥10） were 0. 010 0 -0. 137 0 mg/kg. The average recoveries of ten phenols from 3 typical textile matrices including cotton, wool and ramie, at three spiked concentration levels were in the range of 81% - 105% with relative standard deviations（RSDs） of 1.7% - 8.5% . The proposed method could be used to identify and detect the 10 phenols simultaneously, which makes it effective in residue surveillance of phenols in textile samples.