建立了气相色谱-质谱测定塑料玩具中乙二醇单乙醚、2-甲氧基乙酸乙酯、苯乙烯、2-乙氧基乙酸乙酯、环己酮、双(2-甲氧基乙基)醚、三甲苯、硝基苯、异佛尔酮9种有机物残留量的方法。不同材质的塑料玩具样品经相应溶剂提取,离心后的澄清溶液经Envi-carb石墨化碳固相萃取小柱净化,旋蒸、氮吹浓缩,甲醇定容,过0.2 μm滤膜后用60 m DB-624色谱柱分离,质谱检测,外标法定量。在优化条件下,乙二醇单乙醚的线性范围为0.5~100 mg/L,苯乙烯、三甲苯和异佛尔酮的线性范围为0.05~100 mg/L,其余化合物的线性范围均为0.1~100 mg/L,各物质相关系数均不小于0.999 5。9种有机物的定量下限(LOQ)为0.1~1.0 mg/kg。在3个加标水平下,除三甲苯的回收率较低外,其余8种物质的平均回收率为70%~94%,方法的相对标准偏差(RSD)为2.8%~6.5%。该方法具有准确、操作简便等特点,可用于玩具中乙二醇单乙醚等9种有机物残留量的检测。
Abstract
A gas chromatography-mass spectrometric(GC-MS) method was developed for the determination of 2-ethoxyethanol, 2-methoxyethyl acetate, styrene, 2-ethoxyethyl acetate, cyclohexanone, bis(2-methoxyethyl)ether, 1,3,5-trimethylbenzene, nitrobenzene and isophorone in toys. The experimental conditions were optimized.Toy sample was extracted with appropriate solvent and followed by centrifugalization,then purified with an Envi-carb solid-phase extraction column.The extract was concentrated, and then determined by GC-MS with the external standard method.The calibration curves were linear in the range of 0.5-100 mg/L for 2-ethoxyethanol, 0.05-100 mg/L for styrene, 1,3,5-trimethylbenzene and isophorone, and 0.1-100 mg/L for rest of the targeted compound.The correlation coefficients were all not less than 0.999 5 and the limits of quantitation of 9 organic compounds ranged from 0.1 mg/kg to 1.0 mg/kg.The average recoveries for eight kinds of the substances at three spiked concentration levels ranged from 70% to 94%, except for 1,3,5-trimethylbenzene with low recovery.The relative standard deviations(RSDs) of the method were in the range of 2.8%-6.5%.The method is accurate and simple, and is suitable for the analysis of 9 organic compound residues in various toys.
关键词
气相色谱-质谱法有机物残留量玩具
Keywords
gas chromatography-mass spectrometry(GC-MS)organic residuestoys