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%。
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
所属栏目 专题报道(高关注物质)
基金项目
收稿日期 2017/10/21
修改稿日期
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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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参考文献
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【2】SONG M, SONG M K, CHOI H S, et al. Identification of genes induced by dibutyl phthalate in human thyroid follicular FTC-238 cells[J]. Toxicology & Environmental Health Sciences, 2012,4(2):80-86.
【3】LI M, WANG X, ZHU J, et al. Toxic effects of polychlorinated biphenyls on cardiac development in zebrafish[J]. Molecular Biology Reports, 2014,41(12):7973-7983.
【4】吴刚,汤富彬,赵珊红,等.加速溶剂萃取-气相色谱测定纺织品中磷酸酯类增塑剂[J].丝绸, 2014,51(3):29-33.
【5】DARWIN D C, TAYLOR R T, JEKNAVORIAN A A, et al. Emulsified comb polymer and defoaming agent composition and method of making same:US 6139623[P]. 2000-10-31.
【6】World Health Orgnization. WHO environmental health criteria 111:Triphenyl phosphate[R]. Geneva:National Institute for Hygienic Sciences, 1991.
【7】USFDA. Code of Federal Regulations 21-109.15. Unvoidable contaminants in food for human consumption and food-packaging material[E/OL].[2017-08-11]. https://www.accessdata.fda.gov/scripts/cdrh/cfdocs/cfcfr/CFRSearch.cfm?fr=109.15.
【8】王利兵.食品包装安全学[M].北京:科学出版社, 2011:132.
【9】(EU)No 10/2011 On plastic materials and articals intended to come into contact with foodstuffs[S].
【10】张飞,郑家概,林钦恒,等.超临界CO2/索氏抽提法测定勺子中14种PAEs[J].食品工业, 2016,37(6):288-291.
【11】GB/T 25001-2010纸,纸板和纸浆7种多氯联苯(PCBs)含量的测定[S].
【12】KHOSRAVI K, PRICE G W. Determination of phthalates in soils and biosolids using accelerated solvent extraction coupled with SPE cleanup and GC-MS quantification[J]. Microchemical Journal, 2015,121:205-212.
【13】OTTONELLO G, FERRARI A, MAGI E. Determination of polychlorinated biphenyls in fish:Optimisation and validation of a method based on accelerated solvent extraction and gas chromatography-mass spectrometry[J]. Food Chemistry, 2014,142(1):327-333.
【14】SALAZAR-BELTRÁN D, HINOJOSA-REYES L, RUIZ-RUIZ E, et al. Determination of phthalates in bottled water by automated on-line solid phase extraction coupled to liquid chromatography with UV detection[J]. Talanta, 2017,168(6):291-297.
【15】GB/T 21911-2008食品中邻苯二甲酸酯的测定[S].
【16】HUO L G, LI H D, ZHAO C L, et al. The determination of PCBs in meat and sea food by GC-QqQ-MS/MS[J]. Food Analytical Methods, 2012,5(6):1481-1491.
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【18】LÓPEZ-JIMÉNEZ F J, RUBIO S, PÉREZ-BENDITO D. Determination of phthalate esters in sewage by hemimicelles-based solid-phase extraction and liquid chromatography-mass spectrometry[J]. Analytica Chimica Acta, 2005,551(1):142-149.
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【20】CHAMKASEM N, LEE S, HARMON T. Analysis of 19 PCB congeners in catfish tissue using a modified QuEChERS method with GC-MS/MS[J]. Food Chemistry, 2016,192(2):900-906.
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【23】唐纲岭,边照阳,杨飞,等.烟用接装纸、内衬纸和卷烟条与盒包装纸中18种邻苯二甲酸酯的测定[J].烟草科技, 2012(9):36-40.
【24】YUE M E, LIN Q, LI Q, et al. Determination of PAEs by integrative coupling method of headspace in-tube microextraction and reverse-flow micellar electrokinetic capillary chromatography[J]. Food Analytical Methods, 2017,10(11):3565-3571.
【25】ZHANG Z M, ZHANG H H, LI J L, et al. Determination of phthalic acid esters in seawater and sediment by solid-phase microextraction and gas chromatography-mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017,45(3):348-356.
【26】JOSH M K S, PRADEEP S, BALACHANDRAN S, et al. Temperature-and solvent-dependent migrations of di (2-ethylhexyl) phthalate, the hazardous plasticizer from commercial PVC blood storage bag[J]. Journal of Polymer Research, 2012,19(7):9915.
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