超高效液相色谱-三重四极杆质谱法同时测定纺织品中30种芳香胺类化合物的含量

Simultaneous Determination of 30 Aromatic Amines in Textiles by Ultra-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

取0.1 g 5 mm×5 mm的纺织品小片,加入17 mL(70±2)℃柠檬酸盐缓冲溶液(pH 6.0),参考GB/T 17592—2011进行还原裂解、萃取、浓缩,加适量甲醇稀释,采用超高效液相色谱-三重四极杆质谱法同时测定30种芳香胺类化合物的含量。以ZORBAX Eclipse Plus C18色谱柱作固定相,不同体积比0.1%(体积分数)甲酸溶液和甲醇的混合溶液作流动相进行梯度洗脱,电喷雾离子源正离子(ESI+)模式电离,外标法定量。结果显示:各目标物的质量浓度在50~2000μg·L^(-1)内和峰面积呈线性关系,检出限(3S/N)为0.05~1.69μg·kg^(-1);按照标准加入法进行回收试验,测定值的相对标准偏差(n=6)为3.0%~7.0%,回收率为60.3%~96.5%。方法用于两个质控样品的分析,测定值和指定值基本一致。

An aliquot(0.1 g)of textile flakes with the size of 5 mm×5 mm was taken,and 17 mL of(70±2)℃citrate buffer solution(pH 6.0)was added.Then the standard of GB/T 17592-2011 was adopted for reduction cracking,extraction,and concentration,and the residue was diluted by an appropriate amount of methanol.The 30 aromatic amines were determined simultaneously by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry.ZORBAX Eclipse Plus C18 chromatographic column was used as stationary phase,mixed solutions of 0.1%(volume fraction)formic acid solution and methanol at different volume ratios were used as mobile phase for gradient elution,positive ion(ESI+)mode of electrospray ion source was used for ionization,and external standard method was used for quantification.It was shown that linear relationships between values of the mass concentration and the peak area of each target were kept in the range of 50-2000μg·L^(-1),with detection limits(3S/N)in the range of 0.05-1.69μg·kg^(-1).Test for recovery was made according to the standard addition method,giving RSDs(n=6)of the determined values in the range of 3.0%-7.0%,and recoveries in the range of 60.3%-96.5%.The proposed method was applied to analysis of 2 quality control samples,and the determined values were basically consistent with the specified values.