同位素稀释-超高效液相色谱-串联质谱法测定纺织品中的六溴环十二烷

高等学校化学学报 ›› 2010, Vol. 31 ›› Issue (3): 473.

同位素稀释-超高效液相色谱-串联质谱法测定纺织品中的六溴环十二烷

马强¹, 白桦¹, 王超¹, 席海为², 马微^3,4, 周新¹, 董益阳¹, 王宝麟¹

1. 中国检验检疫科学研究院, 北京 100123;
2. 北京中医药大学中药学院, 北京 100102;
3. 中国农业大学食品科学与营养工程学院, 北京 100083;
4. 黑龙江出入境检验检疫局, 哈尔滨 150086

收稿日期:2009-11-06 出版日期:2010-03-10 发布日期:2010-03-10
通讯作者: 马强, 男, 博士, 助理研究员, 主要从事消费品中化学危害物质的检测技术及风险分析研究. E-mail: maqiang1129@yahoo.com.cn
基金资助:
中国检验检疫科学研究院基本科研业务费专项资金资助.

Determination of Hexabromocyclododecane in Textiles by Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Qiang^1*, BAI Hua¹, WANG Chao¹, XI Hai-Wei², MA Wei^3,4, ZHOU Xin¹, DONG Yi-Yang¹, WANG Bao-Lin¹

1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
2. College of Chinese Pharmacy, Beijing University of Chinese Medicine, Beijing 100102, China;
3. College of Food Science and Nutritional Engineering, China Agricultural University, Beijing 100083, China;
4. Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150086, China

Received:2009-11-06 Online:2010-03-10 Published:2010-03-10
Contact: MA Qiang. E-mail: maqiang1129@yahoo.com.cn
Supported by:
中国检验检疫科学研究院基本科研业务费专项资金资助.

摘要/Abstract

摘要：

建立了同时测定纺织品中α-,β-,γ-六溴环十二烷的同位素稀释-超高效液相色谱-串联质谱分析方法. 不同类型的纺织品样品采用加速溶剂萃取法, 以正己烷-丙酮(体积比1∶1)混合液为萃取溶剂, 在10.3 MPa和80 ℃下, 静态循环萃取3次, 每次5 min, 萃取液经ENVI-CarbⅡ/PSA固相萃取柱净化, 收集二氯甲烷-正己烷(体积比2∶3)洗脱液, 采用Waters ACQUITY UPLC BEH Phenyl色谱柱(50 mm×2.1 mm, 1.7 μm), 以甲醇-水为流动相梯度洗脱分离后进行UPLC/MS/MS多反应监测模式下的定性及定量分析. 结果表明, α-,β-,γ-六溴环十二烷的方法定量限为0.5 μg/kg, 在0.5~10 μg/kg浓度范围内, 低、中及高3个添加水平的平均回收率为84.2%~93.7%, 日内精密度均小于10%, 日间精密度均小于12%. 本方法准确快速, 且灵敏度高, 可用于纺织品的实际检验.

关键词: 同位素稀释; 超高效液相色谱-串联质谱; 纺织品; 六溴环十二烷

Abstract:

A comprehensive analytical method based on isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry has been developed for the determination of α-,β-,γ-hexabromocyclododecane in textiles. Various textile samples were extracted under 10.3 MPa and 80 ℃ by accelerated solvent extraction method with two static cycles using hexane-acetone(1∶1, volume ratio) as the extraction solvent. The reconstructed solution was then cleaned up by ENVI-CarbⅡ/PSA solid phase extraction cartridge. Qualitative and quantitative analysis was carried out for the analyte under the MRM mode after the chromatographic separation on Waters ACQUITY UPLC BEH phenyl(50 mm×2.1 mm, 1.7 μm) column with methanol-water gradient elution. The limit of quantitation(LOQs) for α-,β-,γ-hexabromocyclododecane was 0.5 μg/kg. The mean recoveries at the three spiked levels of 0.5—10 μg/kg were 84.2%—93.7%, with the intra-day precision less than 10% and the inter-day precision less than 12%. This method is accurate, rapid, sensitive and adapt to the inspection of hexabromocyclododecane in textiles.

Key words: Isotope dilution; Ultra performance liquid chromatography-tandem mass spectrometry; Textiles; Hexabromocyclododecane

TrendMD:

马强, 白桦, 王超, 席海为, 马微, 周新, 董益阳, 王宝麟. 同位素稀释-超高效液相色谱-串联质谱法测定纺织品中的六溴环十二烷. 高等学校化学学报, 2010, 31(3): 473.

MA Qiang*, BAI Hua, WANG Chao, XI Hai-Wei, MA Wei, ZHOU Xin, DONG Yi-Yang, .... Determination of Hexabromocyclododecane in Textiles by Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry. Chem. J. Chinese Universities, 2010, 31(3): 473.

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