Determination of Residual Amounts of Quinoline and Isoquinoline in Textiles by Gas Chromatography-Mass Spectrometry
摘 要
称取剪碎的纺织品样品1.000 g,用甲苯10.0 mL于常温下超声提取60 min,用注射器移取部分提取液,经0.45 μm聚四氯乙烯滤膜过滤,取滤液按仪器工作条件进行气相色谱-质谱法分析。以DB-5MS色谱柱(30 m×0.25 mm,0.25 μm)为分离柱,在80~200℃之间以12℃·min-1的升温速率进行色谱分离。在此条件下可使喹啉与异喹啉完全分离。质谱测定中,采用电子轰击离子源(EI)和全扫描模式定性和选择离子扫描模式定量。上述2种化合物均在10.0~250.0 μg·L-1内与其对应峰面积呈线性关系,其检出限均为0.1 mg·kg-1。以空白样品为基体,在3个浓度水平上加入标准溶液进行回收试验,测得喹啉的回收率为82.9%~92.0%,异喹啉的回收率为85.5%~98.1%,2种化合物测定值的平均相对标准偏差(n=6)依次为2.5%,3.1%。应用所提出的方法分析了纺织品实际样品22个,其中有5个试样检出有此2种化合物存在,其质量分数为1.2~27.8 mg·kg-1,均低于OEKO-TEX® STANDARD 100,2019中的规定限量(50 mg·kg-1)。
Abstract
1.000 g of the cut textile sample was ultrasoni-extracted with 10.0 mL of toluene at normal temperature for 60 min. An aliquot of the extract was taken with an injector and filtered through 0.45 μm PTCE filtering membrane, and the filtrate was used for gas chromatography-mass spectrometry analysis under the instrumental working condition. DB-5MS chromatographic column (30 m×0.25 mm, 0.25 μm) was used as the separation column on which quinoline and isoquinoline were well separated by passing the filtrate through it with the column temperature raising at a rate of 12℃·min-1 from 80℃ to 220℃. EI and identifying be whole scanning, quantifying by selected ion scanning were adopted in MS determination. Linear relationships between values of peak areas found and the respective mass concentrations of quinoline and isoquinoline were obtained in the range of 10.0-250.0 μg·L-1. The detection limits found for the 2 compounds were same as 0.1 mg·kg-1. Tests for recovery were made by addition of standard solutions at 3 concentration levels to blank samples and analyzed by the proposed method. Values of recovery in the range of 82.9%-92.0% and 85.5%-98.1% were found for the 2 compounds respectively. Average values of RSDs (n=6) found were 2.5% and 3.1% respectively. 22 samples of textiles were analyzed by the present method, and 5 samples were found to contain quinoline and isoquinoline in the mass fraction range of 1.2-27.8 mg·kg-1, which were much lower than the limitation value of 50 mg·kg-1 as given by the OEKO-TEX® STANDARD 100, 2019 (50 mg·kg-1).
中图分类号 O657.73 DOI 10.11973/lhjy-hx202004009
所属栏目 工作简报
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收稿日期 2019/8/6
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备注保琦蓓,高级工程师,博士,研究方向为环境与消费品中有毒有害物质的检测与研究,baoqibei@126.com
引用该论文: BAO Qibei,MAO Yingjun,SHEN Boyin,QIAN Dan. Determination of Residual Amounts of Quinoline and Isoquinoline in Textiles by Gas Chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(4): 423~427
保琦蓓,毛英俊,沈波音,钱丹. 气相色谱-质谱法测定纺织品中喹啉及其同分异构体异喹啉的残留量[J]. 理化检验-化学分册, 2020, 56(4): 423~427
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