GC-MS Determination of 1,2-Benzene Dicarboxylic Acid-Dialkyl Esters in Plastic Products
摘 要
建立了测定塑料制品中1,2-苯二酸-二(C6-8支链)烷基酯(富C7)(DIHP)和1,2-苯二酸-二(C7-11支链与直链)烷基(醇)酯(DHNUP)含量的气相色谱-质谱法。以乙酸乙酯20 mL为提取剂提取样品(0.500 0 g),于100℃微波萃取30 min,取提取液2.0 mL用乙酸乙酯定容至5.0 mL,过滤后,在选择离子监测(SIM)模式下扫描,用气相色谱-质谱法进行测定,以特征碎片离子的丰度比定性,外标法定量。结果表明,DIHP和DHNUP的线性范围均为0.40~4.0 mg·L-1,检出限(3S/N)为1.0~2.0 mg·kg-1。按标准加入法进行回收试验,回收率在88.6%~115%之间,相对标准偏差(n=6)均小于5.0%。
Abstract
A method for the determination of DIHP and DHNUP in plastic products by gas chromatography-mass spectrometry (GC-MS) was proposed. DIHP and DHNUP in the sample (0.500 0 g) were extracted by microwave extraction at 100℃ for 30 min using 20 mL of ethyl acetate as extraction solvent, and then 2.0 mL of the extract was taken, made its volume up to 5.0 mL with ethyl acetate and filtrated. DIHP and DHNUP were analyzed by GC-MS under selected ion monitor (SIM) mode. The abundance ratio of the characteristic fragment ions was adopted for qualitative analysis, and the external standard method was adopted for quantification. As shown by the results, linear ranges of DIHP and DHNUP were both 0.40-4.0 mg·L-1, with detection limits (3S/N) ranged from 1.0 mg·kg-1 to 2.0 mg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 88.6%-115%, with RSDs (n=6) all less than 5.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201804015
所属栏目 工作简报
基金项目 2014年度安徽省地方标准制修订项目;2015年阜阳市科技计划项目
收稿日期 2017/3/27
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备注王桂苓,工程师,主要从事产品质量检测,wangguil-ing0536@126.com
引用该论文: WANG Guiling,LIANG Yongming,LIU Beibei. GC-MS Determination of 1,2-Benzene Dicarboxylic Acid-Dialkyl Esters in Plastic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(4): 449~454
王桂苓,梁永明,刘贝贝. 气相色谱-质谱法测定塑料制品中1,2-苯二酸-二烷基酯类的含量[J]. 理化检验-化学分册, 2018, 54(4): 449~454
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参考文献
【1】European Chemical Agency (ECHA). (2011) Annex XV dossier:Proposal for identification of a substance as a category 1A or 1B CMR, PBT, vPvB or a substance of an equivalent level of concern[EB/OL]. (2011-05-05)[2015-08-16]. http://echa.europa.eu/doc/consultations/svhc/svhcaxvrepechacmrDIHP.pdf.
【2】European Chemicals Bureau (ECB). Diisoheptyl phthalate. IUCLID dataset. European Commission[EB/OL].[2015-08-16]. http://www.epa.gov/hpv/pubs/summaries/benzene/c13467rr3p.pdf.
【3】ECB 2000. IUCLID dataset for 1,2-Benzenedicarboxylic acid, di-C7-11-branched and linea alkyl esters[EB/OL].[2015-08-16]. http://ecb.jrc.it/iuclid-datasheet/68515424.pdf.
【4】朱曼洁.气相色谱/三重四极杆质谱(TSQ8000)用于食品中19种邻苯二甲酸酯的检测分析[J].中国食品, 2014(3):54-57.
【5】徐善浩,邬蓓蕾,袁丽凤,等.气相色谱-质谱法测定洗涤用品中6种邻苯二甲酸酯[J].理化检验-化学分册, 2016,52(3):271-274.
【6】马军,滕应,马文亭,等.层析净化-气相色谱-质谱法测定烟叶中6种邻苯二甲酸酯[J].理化检验-化学分册, 2016,52(4):392-396.
【7】GB/T 21928-2008食品塑料包装材料中邻苯二甲酸酯的测定[S].
【8】GB/T 22048-2015玩具及儿童用品中特定邻苯二甲酸酯增塑剂的测定[S].
【9】SN/T 1779-2006塑料血袋中邻苯二甲酸酯类增塑剂的测定气相色谱串联质谱法[S].
【10】SN/T 2249-2009塑料及其制品中邻苯二甲酸酯类增塑剂的测定气相色谱-质谱法[S].
【11】薛建平,任学勤,裴德君,等.超声萃取-气质联用法测定纺织品中的2种邻苯二甲酸酯[J].印染助剂, 2014,31(12):46-49.
【2】European Chemicals Bureau (ECB). Diisoheptyl phthalate. IUCLID dataset. European Commission[EB/OL].[2015-08-16]. http://www.epa.gov/hpv/pubs/summaries/benzene/c13467rr3p.pdf.
【3】ECB 2000. IUCLID dataset for 1,2-Benzenedicarboxylic acid, di-C7-11-branched and linea alkyl esters[EB/OL].[2015-08-16]. http://ecb.jrc.it/iuclid-datasheet/68515424.pdf.
【4】朱曼洁.气相色谱/三重四极杆质谱(TSQ8000)用于食品中19种邻苯二甲酸酯的检测分析[J].中国食品, 2014(3):54-57.
【5】徐善浩,邬蓓蕾,袁丽凤,等.气相色谱-质谱法测定洗涤用品中6种邻苯二甲酸酯[J].理化检验-化学分册, 2016,52(3):271-274.
【6】马军,滕应,马文亭,等.层析净化-气相色谱-质谱法测定烟叶中6种邻苯二甲酸酯[J].理化检验-化学分册, 2016,52(4):392-396.
【7】GB/T 21928-2008食品塑料包装材料中邻苯二甲酸酯的测定[S].
【8】GB/T 22048-2015玩具及儿童用品中特定邻苯二甲酸酯增塑剂的测定[S].
【9】SN/T 1779-2006塑料血袋中邻苯二甲酸酯类增塑剂的测定气相色谱串联质谱法[S].
【10】SN/T 2249-2009塑料及其制品中邻苯二甲酸酯类增塑剂的测定气相色谱-质谱法[S].
【11】薛建平,任学勤,裴德君,等.超声萃取-气质联用法测定纺织品中的2种邻苯二甲酸酯[J].印染助剂, 2014,31(12):46-49.
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