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气相色谱-质谱法测定烟用接装纸中的邻苯二甲酸酯、磷酸三丁酯和多氯联苯
          
Determination of Phthalate Esters, Tributyl Phosphate and Polychlorinated Biphenyls in Tipping Paper for Cigarette by Gas Chromatography-Mass Spectrometry

摘    要
称取0.500 0 g的样品,加入10 mL去离子水,振荡15 min,使水充分浸润样品;加入10 mL乙醇,500 μL的100 mg·L-1 D4-邻苯二甲酸二丁酯和28 mg·L-1 2,4,6-三溴联苯的混合内标溶液,超声提取30 min;加入4 g MgSO4,1 g NaCl,涡旋后取2 mL上清液,加入5 mL正己烷-乙酸乙酯(3+2)混合液进行液液萃取;采用DB-5MS UI毛细管色谱柱(30 m×0.25 mm,0.25 μm)分离提取液中的18种邻苯二甲酸酯、磷酸三丁酯和7种多氯联苯,质谱中采用电子轰击离子源和选择离子监测模式。26种化合物的峰面积与内标峰面积的比值与对应的质量浓度之比在一定范围内呈线性关系,检出限(3S/N)在0.010~2.558 mg·kg-1之间。加标回收率在85.1%~102%之间,测定值的相对标准偏差(n=6)小于9.0%。
标    签 邻苯二甲酸酯   磷酸三丁酯   多氯联苯   液液提取   气相色谱-质谱法   烟用接装纸   phthalate ester   tributyl phosphate   polychlorinated biphenyl   liquid-liquid extraction   gas chromatography-mass spectrometry   tipping paper for cigarette  
 
Abstract
The sample (0.500 0 g) was added in to 10 mL of deionized water, and the mixture was shaken for 15 min to make the water fully infiltrate the sample. Then 10 mL of ethanol, 500 μL of mixed internal standard solution containing 100 mg·L-1 D4-dibutyl phthalate and 28 mg·L-1 2,4,6-tribromobiphenyl were added, and the mixtrue was ultrasonically extracted for 30 min. After adding 4 g of MgSO4, 1 g of NaCl, the mixture was vortexed. Then 2 mL of supernatant was taken, and 5 mL of a mixture of n-hexane-ethyl acetate (3+2) was added for liquid-liquid extraction. 18 kinds of phthalate esters, tributyl phosphate, and 7 kinds of polychlorinated biphenyls in the extract were separated on a DB-5MS UI capillary column (30 m×0.25 mm, 0.25 μm). Electron bombardment ion source and selective ion monitoring mode were selected in MS analysis. The ratios of the peak areas of the 26 compounds to the peak areas of the internal standards were linear with the corresponding rations of mass concentrations within definite ranges, and the detection limits (3S/N) were in the range of 0.010-2.558 mg·kg-1. Values of recovery obtained by standard addition method ranged from 85.1% to 102%, and RSDs (n=6) were less than 9.0%.

中图分类号 O657.63   DOI 10.11973/lhjy-hx201809023

 
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所属栏目 专题报道(高关注物质)

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收稿日期 2017/10/21

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备注王颖,高级工程师,硕士,主要从事烟草、烟气及烟用材料的化学检验工作,carobit@163.com

引用该论文: WANG Ying,BIAN Zhaoyang,LI Zhonghao,TANG Gangling,YANG Fei,LIU Shanshan,DENG Huimin. Determination of Phthalate Esters, Tributyl Phosphate and Polychlorinated Biphenyls in Tipping Paper for Cigarette by Gas Chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(9): 1092~1100
王颖,边照阳,李中皓,唐纲岭,杨飞,刘珊珊,邓惠敏. 气相色谱-质谱法测定烟用接装纸中的邻苯二甲酸酯、磷酸三丁酯和多氯联苯[J]. 理化检验-化学分册, 2018, 54(9): 1092~1100


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