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气相色谱-质谱法测定塑料中7种有机磷酸酯阻燃剂的含量
          
GC-MS Determination of 7 Organophosphate Ester Flame Retardants in Plastic

摘    要
样品0.100 0 g置于微波萃取管中,加入乙腈15 mL,涡流振荡2 min,微波萃取20 min,冷却至室温后,收集上清液。再加入乙腈10 mL涡流振荡2 min,合并上清液。所得萃取液蒸发至近干,再用氮气吹干,用10 mL丙酮稀释。以DB-5MS色谱柱为固定相,采用气相色谱-质谱法测定上述溶液中三(2-氯乙基)磷酸酯、三(1,3-二氯丙基)磷酸酯、三(2-氯异丙基)磷酸酯、磷酸三苯酯、磷酸三对甲苯酯、磷酸三间甲苯酯和磷酸三邻甲苯酯等7种有机磷酸酯阻燃剂的含量。质谱分析中采用选择离子监测(SIM)模式。7种有机磷酸酯阻燃剂的线性范围均为1.00~100 mg·L-1,测定下限(10S/N)为0.28~1.00 mg·L-1。按标准加入法进行回收试验,回收率在85.9%~95.2%之间,相对标准偏差(n=9)均小于8.0%。
标    签 气相色谱-质谱法   微波萃取   有机磷酸酯阻燃剂   塑料   GC-MS   microwave extraction   organophosphate ester flame retardant   plastic  
 
Abstract
The sample (0.100 0 g) was placed into the microwave extraction tube, and 15 mL of acetonitrile was added. The mixture was oscillated whirling for 2 min and extracted by microwave for 20 min. Cooling to room temperature, the supernatant was collected. 10 mL of acetonitrile was added and the mixture was oscillated whirling for 2 min. The above supernatants were combined and concentrated to dryness nearby, and then dried by N2-blowing. The residue was diluted with 10 mL of acetone. Tris(2-chloroethyl) phosphate, tris(1,3-dicloropropyl) phosphate, tris(2-chloroisopropyl) phosphate, triphenyl phosphate, tri-p-cresyl phosphate, tri-m-cresyl phosphate and tri-o-cresyl phcsphate in the above solution were determined by gas chromatography mass spectrometry (GC-MS) using DB-5MS column as the stationary phase.SIM mode was adopted in MS analysis. Linearity ranges of the 7 organophosphate ester flame retardants were all 1.00-100 mg·L-1, with lower limits of determination (10S/N) of 0.28-1.00 mg·L-1.Test for recovery was made by standard addition method, giving results in the range of 85.9%-95.2%, with RSDs (n=9) all less than 8.0%.

中图分类号 O657.63   DOI 10.11973/lhjy-hx201801013

 
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所属栏目 工作简报

基金项目 国家质量监督检验检疫总局科研项目(2015IK053)

收稿日期 2017/1/5

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备注周小丽(1979-)女,河北石家庄人,高级工程师,主要从事各种消费品中有毒有害物质研究工作,zhouxiaoli204@163.com

引用该论文: ZHOU Xiaoli,GUO Heng,LI Qin,LI Jinguang. GC-MS Determination of 7 Organophosphate Ester Flame Retardants in Plastic[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(1): 64~68
周小丽,郭珩,李芹,李劲光. 气相色谱-质谱法测定塑料中7种有机磷酸酯阻燃剂的含量[J]. 理化检验-化学分册, 2018, 54(1): 64~68


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参考文献
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【8】赵岩,张艳艳,高永刚,等.超声萃取/气相色谱-质谱法测定电子电气中6种禁用有机磷阻燃剂[J].现代测量与实验室管理, 2016,24(3):3-8.
 
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