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机构地区:[1]国家纺织服装产品质量监督检验中心(福建),福建福州350026 [2]福建省纤维检验局,福建福州350026
出 处:《分析测试学报》2014年第4期427-431,共5页Journal of Instrumental Analysis
基 金:国家质检总局科技计划项目(2012QK046)
摘 要:建立了气相色谱-质谱联用(GC-MS)测定纺织品中1,2-二氯乙烷的方法.样品经甲醇超声提取后,以TG-624(30 m×0.32 mm×1.8 μm)为色谱柱,采用气相色谱-质谱联用全扫描和选择离子扫描进行定性定量分析、外标法定量.结果表明:在0.05~30 mg/L范围内,1,2-二氯乙烷的线性关系良好,相关系数为0.999 3;方法检出限为0.50 mg/kg.在0.5、1.0、5.0 mg/kg 3个加标水平下,粘纤、聚酯、羊毛、锦纶、桑蚕丝、腈纶、棉7种纺织品基底的加标回收率为85.2% ~ 101.4%,相对标准偏差(RSD)为4.0%~7.4%.该方法简便、准确,灵敏度和精密度高,适用于纺织品中1,2-二.氯乙烷的分析检测.A gas chromatography - mass spectrometric ( GC - MS) method was developed for the de- termination of 1, 2-dichloroethane in textiles. The samples were extracted with methanol under ultra- sonic assistance. The separation and quantification of 1, 2-dichloroethane were achieved on an TG - 624 column ( 30 m x 0. 32 mm x 1.8 μm) using temperature programming. The identification and quantification of 1, 2-dichloroethane were performed by GC - MS under full scan and selected ion monitoring scan with the external standard method. The result indicated that the calibration curve showed a good linear relationship between peak area and concentration of 1, 2-dichloroethane in the range of 0.05 - 30 mg/L, with a correlation coefficient of 0. 999 3. The limit of detection was 0.50 mg/kg. The average recoveries of 1, 2-dichloroethane from 7 typical textile matrices including vis- cose fiber, polyester, wool, nylon, ramie, polyacrylonitrile fiber and cotton, at three spiked con- centration levels of 0. 5, 1.0, 5.0 mg/kg were in the range of 85.2% - 101.4% with relative stand- ard deviations (RSDs) of 4. 0% - 7.4%. With the advantages of low detection limit, good accuracy and high precision, the method could be used for residue surveillance of 1, 2-dichloroethane in tex- tile samples.
关 键 词:纺织品 1 2-二氯乙烷 气相色谱-质谱联用法 gas chromatography-mass SPECTROMETRY (GC-MS)
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