摘要
建立了同时快速测定纺织品中8种多环芳烃的气相色谱-质谱联用（GC-MS）方法。样品经正己烷-丙酮（1∶1）超声波提取,氮吹浓缩后采用DB-17MS色谱柱程序升温分离,选择离子模式采集,外标法定量。研究了纺织品中8种多环芳烃的提取方法,并对色谱和质谱条件进行了优化。实验结果表明,多环芳烃的浓度在0.05-1.00 mg/L或0.10-1.00 mg/L范围内与峰面积呈良好的线性关系,相关系数（r^2）均大于0.995,方法检出限（LOD）为0.02-0.05 mg/kg,方法定量下限（LOQ）为0.05-0.10 mg/kg。在3个加标水平下的回收率为81.2%-106.4%,相对标准偏差（RSD）为2.5%-8.5%。该方法灵敏度高,操作简便,定量准确,适用于纺织品中8种多环芳烃的分析测定。
A rapid analytical method based on gas chromatography-mass spectrometry（GC-MS）was established for the simultaneous determination of eight polycyclic aromatic hydrocarbons（PAHs）in textiles.PAHs in the samples were extracted with hexane-acetone（1 ∶ 1） by ultrasonic technique,followed by concentrated with nitrogen.The separation was performed on a DB-17 MS capillary column with temperature programming.The identification was performed by GC-MS in selected ion monitoring（SIM） mode,and the quantification was carried out by the external standard method.The processes of extraction were investigated,and the GC-MS parameters were optimized.The calibration curves of eight PAHs showed good linearities in the ranges of 0.05-1.00 mg / L or 0.10-1.00 mg / L with correlation coefficients（r^2） larger than 0.995.The limits of detection（LOD） of PAHs in textiles ranged from 0.02 mg / kg to 0.05 mg / kg and the limits of quantitation（LOQ） ranged from 0.05 mg / kg to 0.10 mg / kg.The average recoveries of eight PAHs at three spiked concentrtion levels were in the range of 81.2%-106.4% with relative standard deviations（RSDs,n = 6） of 2.5%-8.5%.The method was suitable for the simultaneous determination of eight PAHs in textiles with high accuracy,easy operation and good precision.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第4期443-447,共5页
Journal of Instrumental Analysis
基金
国家质量监督检验检疫总局科技计划项目(2014QK027)
关键词
气相色谱-质谱联用法(GC-MS)
纺织品
多环芳烃
测定
gas chromatography-mass spectrometry（GC-MS）
textile
polycyclic aromatic hydrocarbon
determination
