扫一扫 加微信
首页 > 期刊论文 > 论文摘要
超声提取-气相色谱-质谱法测定塑料快递包装中6种邻苯二甲酸酯类增塑剂的含量
          
Determination of 6 Phthalate Esters in Plastic Express Package by Gas Chromatography-Mass Spectrometry with Ultrasonic Extraction

摘    要
鉴于现用标准的前处理方式存在操作复杂、耗时较长及设备昂贵等问题,选用易于实现的超声提取技术,通过考察不同提取条件对质控样中邻苯二甲酸酯(PAEs)类增塑剂提取效果的影响,提出了超声提取-气相色谱-质谱法测定塑料快递包装中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁苄酯(BBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)和邻苯二甲酸二异癸酯(DIDP)等6种PAEs类增塑剂含量的方法。将塑料包装样品剪成小块,称取0.5 g于玻璃萃取瓶中,加入20 mL二氯甲烷,于25℃超声30 min,上清液经0.45 μm有机滤膜过滤,再加入一定量的邻苯二甲酸二戊酯(内标)溶液,使其质量浓度为5.0 mg·L-1。6种PAEs在DB-5MS毛细管色谱柱上以柱升温程序的方式进行分离,用配有电子轰击离子源的质谱仪以全扫描方式进行检测,内标法定量。结果显示:6种PAEs标准曲线的线性范围为0.10~5.0 mg·L-1(DBP、BBP、DEHP和DNOP)和1.0~50 mg·L-1(DINP和DIDP),检出限(3S/N)为0.03~0.63 mg·kg-1;对空白样品进行加标回收试验,6种PAEs的回收率为92.2%~105%,测定值的相对标准偏差(n=6)为0.76%~3.2%;方法用于10个塑料快递包装样品分析,除两种样品检出DBP和DEHP外,其他样品中均未检出目标物;对比了超声提取法、索氏提取法(GB/T 22048-2015)和微波消解法(SN/T 2249-2009)对质控样和实际样品测定结果的影响,质控样的测定结果均在认定值的不确定度范围内,实际样品中有3个样品检出DBP和DEHP,其余样品中均为未检出目标物,并且这3种前处理方式所得结果接近。
标    签 邻苯二甲酸酯   气相色谱-质谱法   超声提取   塑料快递包装   phthalate ester   gas chromatography-mass spectrometry   ultrasonic extraction   plastic express package  
 
Abstract
In view of the problems of complex operation, long time consuming and expensive equipment in the pretreatment methods adopted by current standards, ultrasonic extraction technology, which was easy to implement, was selected. The effects of different extraction conditions on the extraction effect of phthalate esters (PAEs) in the quality control sample was investigated, and a method for the determination of 6 PAEs, including dibutyl phthalated (DBP), butyl benzyl phthalate (BBP), bis (2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-iso-nonyl phthalate (DINP) and di-iso-decyl phthalate (DIDP) in plastic express package by gas chromatography-mass spectrometry with ultrasonic extraction was proposed. The plastic package sample was cut into small pieces, and 0.5 g of an aliquot and 20 mL of methylene chloride were added into a glass extraction bottle, and ultrasonic extraction was performed for 30 min at 25℃. The supernatant was filtered by 0.45 μm organic filter membrane, and a certain amount of dipentyl phthalate (internal standard) solution was added to make its mass concentration to 5.0 mg·L-1. The 6 PAEs were separated on DB-5MS capillary column with column temperature program, detected by mass spectrometer equipped with electron impact ionization and full scanning mode, and quantified by internal standard method. It was shown that the linear ranges of standard curves of 6 PAEs were 0.10-5.0 mg·L-1 (DBP, BBP, DEHP and DNOP) and 1.0-50 mg·L-1 (DINP and DIDP), with detection limits (3S/N) in the range of 0.03-0.63 mg·kg-1. Test for recovery was made on blank sample by addition standard method, giving results of 6 PAEs in the range of 92.2%-105%, and RSDs (n=6) of the determined values were ranged from 0.76% to 3.2%. This method was applied to the analysis of 10 plastic express package samples, DBP and DEHP were detected in two samples, and the targets were not detected in the other samples. The effects of ultrasonic extraction method, Soxhlet extraction method (GB/T 22048-2015) and microwave digestion method (SN/T 2249-2009) on the determined results of the quality control sample and actual samples were compared, and the determined results of the quality control sample were within the uncertainty ranges of the certified values. DBP and DEHP were detected in 3 actual samples, the targets were not detected in the other samples, and the results obtained by the 3 pretreatment methods were similar.

中图分类号 O675.63   DOI 10.11973/lhjy-hx202210007

 
  中国光学期刊网论文下载说明


所属栏目 工作简报

基金项目

收稿日期 2021/3/18

修改稿日期

网络出版日期

作者单位点击查看

备注英琪,工程师,硕士,从事邮政用品用具检测及邮政标准化研究,yingqi@chinapost.com.cn

引用该论文: YING Qi,HUANG Yanan,ZHAO Zhenzhen,HE Shi,GAO Xiaoqing. Determination of 6 Phthalate Esters in Plastic Express Package by Gas Chromatography-Mass Spectrometry with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(10): 1159~1164
英琪,黄亚楠,赵真真,何石,高晓庆. 超声提取-气相色谱-质谱法测定塑料快递包装中6种邻苯二甲酸酯类增塑剂的含量[J]. 理化检验-化学分册, 2022, 58(10): 1159~1164


论文评价
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
分享论文
分享到新浪微博 分享到腾讯微博 分享到人人网 分享到 Google Reader 分享到百度搜藏分享到Twitter

参考文献
【1】SU T C, HWANG J S, TORNG P L, et al. Phthalate exposure increases subclinical atherosclerosis in young population[J]. Environmental Pollution, 2019,250:586-593.
 
【2】HEUDORF U, MERSCH-SUNDERMANN V, ANGERER J. Phthalates:Toxicology and exposure[J]. International Journal of Hygiene and Environmental Health, 2007,210(5):623-634.
 
【3】WITTASSEK M, KOCH H M, ANGERER J, et al. Assessing exposure to phthalates-The human biomonitoring approach[J]. Molecular Nutrition & Food Research, 2011,55(1):7-31.
 
【4】HUELSMANN R D, WILL C, CARASEK E. Novel strategy for disposable pipette extraction (DPX):Low-cost Parallel-DPX for determination of phthalate migration from common plastic materials to saliva simulant with GC-MS[J]. Talanta, 2021,221:121443.
 
【5】刘芳卫,英琪,赵真真,等.气相色谱-质谱法测定快递封装用品中塑化剂含量[J].中国标准化, 2020(增刊1):393-396.
 
【6】樊诗亮,何丽芝,陆扣萍,等.土壤中邻苯二甲酸脂提取与检测方法的研究进展[J].环境污染与防治, 2016,38(6):81-87.
 
【7】刘成霞,朱洋,刘绿叶.高效液相色谱法测定土壤中6种邻苯二甲酸酯的含量及其生物有效性的评价[J].理化检验-化学分册, 2020,56(2):206-210.
 
【8】白亚敏,杨小珊,毛庆,等.液相色谱-质谱法测定化妆品中10种邻苯二甲酸酯[J].日用化学工业, 2014,44(8):472-475.
 
【9】祝伟霞,刘亚风,袁萍,等.液相色谱-串联质谱法测定纺织品中18种邻苯二甲酸酯类化合物[J].理化检验-化学分册, 2013,49(2):156-160.
 
【10】莫玲,胡银川,蔡小先,等.塑料包装材料中邻苯二甲酸酯的LC/MS/MS测定方法研究[J].中国酿造, 2013,32(9):135-138.
 
【11】张国民,温素素.气相色谱-质谱法测定食品中17种邻苯二甲酸酯类塑化剂的含量[J].理化检验-化学分册, 2020,56(1):46-54.
 
【12】周天啸,高俊伟,彭姚珊,等.气相色谱-串联质谱法测定纸质及塑料食品包装材料中12种多环芳烃的含量[J].理化检验-化学分册, 2016,52(12):1388-1393.
 
【13】李志伟,纪朋,马慧丽.塑料中邻苯二甲酸酯类化合物的GC/MS分析方法[J].郑州轻工业学院学报(自然科学版), 2009,24(5):12-15.
 
【14】綦敬帅,宋吉英,史衍玺,等.用索氏提取-气相色谱法测定PVC管材中的邻苯二甲酸酯类增塑剂[J].塑料科技, 2014,42(2):100-105.
 
【15】焦艳娜,丁利,肖家勇,等.气相色谱-质谱法同时测定塑料包装材料中多种有毒有害物质[J].食品安全质量检测学报, 2013,4(4):981-987.
 
【16】王学连,周立,张丹青,等.GC-MS测试PVC制品中的23种邻苯二甲酸酯类增塑剂[J].广州化工, 2020,48(6):104-106.
 
【17】方丽,林泽鹏,林晨,等.气质联用法测定食品包装材料中22种邻苯二甲酸酯残留方法的探讨[J].食品工业, 2015,36(1):291-296.
 
【18】国家市场监督管理总局,国家标准化管理委员会.绿色产品评价 快递封装用品:GB/T 39084-2020[S].北京:中国标准出版社, 2020.
 
相关信息
   标题 相关频次
 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
 4
 超声提取-气相色谱-质谱法测定薄荷型卷烟烟丝及滤嘴中薄荷醇的含量
 3
 Carb/NH2固相萃取柱净化-气相色谱-质谱法测定乳粉中二苯胺的残留量
 2
 层析净化-气相色谱-质谱法测定烟叶中6种邻苯二甲酸酯
 2
 茶叶中29种挥发性有机物的固相微萃取-气相色谱-质谱法测定及其危害水平评估
 2
 超高效液相色谱法测定烟用水基胶中3种异噻唑啉酮杀菌剂
 2
 超声波萃取与索氏萃取丙烯腈-丁二烯-苯乙烯中四溴双酚A的比较研究
 2
 超声萃取分离-气相色谱-质谱法测定土壤中的3种酰胺类化合物含量
 2
 超声萃取-冷蒸气-原子荧光光谱法测定沉积物和土壤样品中甲基汞
 2
 超声萃取-气相色谱-质谱法测定卷烟主流烟气中的6种挥发酚
 2
 超声萃取-三氟乙酰胺衍生化气相色谱-质谱法测定血液中阿片类毒品
 2
 超声提取-超高效液相色谱-串联质谱法测定毛发中常见毒品及代谢物的含量
 2
 超声提取-电感耦合等离子体质谱法快速测定海蜇制品中铝的残留量
 2
 超声提取-动态液相微萃取-气相色谱法测定土豆中有机磷农药
 2
 超声提取-分光光度法测定大黄中总蒽醌类化合物
 2
 超声提取-高效液相色谱-电感耦合等离子体质谱法测定水产品中5种形态的砷
 2
 超声提取-高效液相色谱法测定粗榧中高三尖杉酯碱
 2
 超声提取-高效液相色谱法测定纺织品中5种同分异构CMR物质
 2
 超声提取-高效液相色谱法测定土壤中联苯胺的含量
 2
 超声提取-连续流动分析法测定卷烟纸中钙的含量
 2
 超声提取-凝胶渗透色谱法净化-超高效液相色谱-串联质谱法测定鸭肠及其制品中6种常见抗生素的残留量
 2
 超声提取-气相色谱法测定保健品中15种有机氯农药残留量
 2
 超声提取-气相色谱法同时测定稻谷中18种有机氯农药和7种多氯联苯
 2
 超声提取-气相色谱-质谱法测定美缝剂中壬基酚的含量
 2
 超声提取-石墨炉原子吸收光谱法测定高纯石墨中铅的含量
 2
 超声提取-石墨炉原子吸收光谱法测定土壤中有效态镉
 2
 吹扫捕集-气相色谱-质谱法测定环境空气和废气中的三甲胺
 2
 吹扫捕集-气相色谱-质谱法测定土壤中28种挥发性有机化合物的含量
 2
 大气降尘中有机物的提取分离及其气相色谱-质谱分析
 2
 顶空固相微萃取-气相色谱-质谱法测定太湖水源水中嗅味物质土臭素、2-甲基异莰醇以及β-紫罗兰酮的含量
 2