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

称取0.500 0g的样品,加入10mL去离子水,振荡15min,使水充分浸润样品;加入10mL乙醇,500μL的100mg·L-1 D4-邻苯二甲酸二丁酯和28mg·L-1 2,4,6-三溴联苯的混合内标溶液,超声提取30min;加入4g MgSO4,1g NaCl,涡旋后取2mL上清液,加入5mL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,0.25μm)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%。

The sample（0.500 0 g）was added in to 10 mL of deionized water,and the mixture was shaken for15 min to make the water fully infiltrate the sample.Then 10 mL of ethanol,500μL 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 polychlorinated biphenyls in the extract were separated on a DB-5 MS UI capillary column（30 m×0.25 mm,0.25μm）.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 corespongding rations of mass concentrations within definite ranges,and the detection limits（3 S/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%.