提出了纺织品中辛基酚(OP)和辛基酚聚氧乙烯醚(OPOE)的高效液相色谱-质谱(HPLC-MS)测定方法。纺织品中的OP和OPOE经甲醇提取,蒸馏浓缩后用甲醇定容。以C18反相色谱柱为分离柱,以甲醇-水(80+20)溶液为流动相洗脱,采用电喷雾离子源检测。OP和OPOE的质量浓度均在0.01~0.5 mg·L-1范围内与峰面积呈线性关系,测定下限(10S/N)分别为0.07,0.05 mg·kg-1。在0.5,1.0,2.0 mg·kg-1 3个浓度水平下进行加标回收试验,OP和OPOE的回收率分别在90.5%~108%和91.4%~109%之间,相对标准偏差(n=7)均小于8%。

A method of HPLC-MS for determination of octylphenol (OP) and octylphenol polyoxyethylene ether (OPOE) in textile was proposed. The OP and OPOE in textile were extracted with methanol; the extract obtained was evaporated and made up to 10 mL with methanol. C18 reversed phase column was used as stationary phase and a mixture of methanol and water (80+20) was used as mobile phase. ESI was adopted in MS. Linear relationships between values of peak area and mass concentration of OP and OPOE were kept in the same range of 0.01-0.5 mg·L-1, with values of lower limit of determination (10S/N) of 0.07 and 0.05 mg·kg-1 respectively. Tests for recovery were made at the concentration levels of 0.5, 1.0 and 2.0 mg·kg-1 of the mixed standards, values of recovery found were in the ranges of 90.5%-108% for OP and 91.4%-109% for OPOE with RSD′s (n=7) less than 8%.