采用液相色谱-串联质谱法测定纺织品中18种邻苯二甲酸酯类化合物。样品经二氯甲烷提取,氮吹至近干后,用甲醇定容至1 mL。在色谱分离中选用Shiseido MG Ⅱ C18色谱柱,5 mmol·L-1乙酸铵甲醇溶液和水按不同比例混合作流动相梯度淋洗。质谱测定中采用正离子模式大气压化学电离源、多反应监测模式测定18种邻苯二甲酸酯类化合物。18种邻苯二甲酸酯类化合物分别在一定的质量浓度范围内呈线性,测定下限(10S/N)在0.1~1.0 mg·kg-1之间。方法用于成人内衣和婴幼儿T恤样品分析,回收率在68.7%~112%之间,测定值的相对标准偏差(n=10)在4.3%~18%之间。

LC-MS/MS was proposed to the determination of 18 phthalates in textiles. The sample was extracted with CH2Cl2, evaporated to dryness by N2-blowing and taken up with 1 mL of CH3OH. Shiseido MG Ⅱ C18 chromatographic column was used as stationary phase, and the mixture of 5 mmol·L-1 ammonium acetate and water in different ratios was used as mobile phase in the gradient elution. The atmospheric pressure chemical ionization source with positive ionization mode as well as MRM mode of detection were adopted in MS/MS determination. Linear relationships between values of peak area and mass concentration of 18 phthalates were kept in definite ranges with lower limits of determination (10S/N) in the range of 0.1-1.0 mg·kg-1. The proposed method was applied to the analysis of samples of adult underwear and infant T-shirts, giving values of recovery in the range of 68.7%-112% and RSD′s (n=10) in the range of 4.3%-18% respectively.