液相色谱-串联质谱法测定纺织品中4种二苯甲酮类紫外吸收剂的最大迁移量

LC-MS/MS Determination of Maximum Migration of 4 Benzophenone-Type UV Absorbers in Textiles

采用液相色谱-串联质谱法测定纺织品中二苯甲酮、2,4-二羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮和2-羟基-4-正辛氧基二苯甲酮等4种二苯甲酮类紫外吸收剂的最大迁移量。采用水、酸性汗液、碱性汗液、皂液等迁移模拟液。迁移模拟液加入到纺织品样品中后,采用水浴摇床振荡,振荡频率为80r·min^(-1),迁移时间为90min,在水及皂液中迁移时水温为常温,在酸性汗液及碱性汗液中迁移时水温为(37±2)℃,迁移模拟液采用乙腈液液萃取。以Waters Atlantis T3色谱柱为分离柱,以不同体积比的乙腈和水的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源和多反应监测模式。4种二苯甲酮类紫外吸收剂的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为1~3μg·L^(-1),测定下限(10S/N)为3~10μg·L^(-1)。以空白样品为基体进行加标回收试验,所得回收率为85.5%~102%,测定值的相对标准偏差(n=6)为4.4%~8.4%。对纺织品样品中4种二苯甲酮类紫外吸收剂进行迁移评估,结果表明:4种二苯甲酮类紫外吸收剂的最大迁移比例为0.02%~3.65%,最大迁移时间为60~90min。

LC-MS/MS was applied to the determination of maximum migration of 4 benzophenone〉type UV absorbers, i.e. BP, UV-0, UV-9 and UV-531 in textiles. Water, acidic sweat, basic sweat and soap lye were used as migration simulants. The textile sample was oscillated in water bath shaker for 90 min with the frequency of 80 r ·min^-1 after adding migration stimulant. Temperature of bath was set at room temperature for water and soap lye, and （37±2）℃ for acidic sweat and basic sweat. The above migration simulants were extracted by liquid-liquid extraction with aeetonitrile. Waters Atlantis T3 chromatographic column was used as stationary phase, and the mixture of aeetonitrile and water mixed in different ratios was used as mobile phase in gradient elution. ESI and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 4 benzophenone-type UV absorbers were kept in definite ranges, with detection limits （3S/N） in the range of 1--3 ~g ~ L 1 and lower limits of determination （10S/N） in the range of 3-10μg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 85.5%-102%, with RSDs （n=6） in the range of 4. 4%-8. 4%. The migration of the 4 benzophenone- type UV absorbers in textile samples was assessed. It was found that the maximum migration ratios of the 4 benzophenone-type UV absorbers were in the range of 0. 02%-3. 65%, and the maximum migration time was in the range of 60-90 min.