顶空-气相色谱-质谱法测定聚酯纤维材质消费品中54种致敏性芳香剂的含量

Determination of 54 Fragrance Allergens in Consumer Products with Polyester Fiber Matrices by Gas Chromatography-Mass Spectrometry with Headspace

样品剪碎后置于顶空瓶中,用丙酮提取,采用顶空-气相色谱-质谱法测定。在色谱分析时,采用HP-35低流失石英毛细管色谱柱作固定相,在程序升温条件下分离54种致敏性芳香剂;在质谱分析时,采用电喷雾离子(EI)源进行电离,选择离子监测模式进行数据采集。结果表明,54种致敏性芳香剂在0.2~50 mg·L^(-1)内和对应的峰面积呈线性关系,测定下限(10s)为0.10~1.52 mg·kg^(-1);按照标准加入法进行回收试验,回收率为78.7%~107%,测定值的相对标准偏差(n=6)为1.9%~11%。方法应用于5批聚酯纤维材质消费品的分析,每批样品中均检出了致敏性芳香剂,检出量为0.319~0.884 mg·kg^(-1)。

The sample was cut into small pieces,placed into a headspace bottle,extracted by cuetone,and determined by gas chromatography-mass spectrometry with headspace.In chromatographic analysis,the HP-35 low loss quartz capillary column was used as the stationary phase to separate 54 fragrance allergens under programmed temperature conditions.In mass spectrometry analysis,the electrospray ion(EI)source was used for ionization,and the selected ion monitoring mode was selected for data collection.It was shown that linear relationships between values of the mass concentration and the corresponding peak area of 54 fragrance allergens were kept in the range of 0.2-50 mg·L^(-1),with lower limits of determination(10s)in the range of 0.10-1.52 mg·kg^(-1).Test for recovery was made according to the standard addition method,giving recoveries in the range of 78.7%-107%,and RSDs(n=6)of the determined values ranged from 1.9%to 11%.The proposed method was applied to the analysis of 5 batches of consumer products with polyester fiber matrices,and fragrance allergens were detected in each batch of sample,with detection amounts ranged from 0.319 mg·kg^(-1)to 0.884 mg·kg^(-1).