高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究

林春梅; 刘莹峰; 张子豪; 李全忠; 李丹; 翟翠萍; 肖前; 郑建国

doi:doi：10.3969/j.issn.1004-4957.2019.03.003

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高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究

- 高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究
- Study on Analysis of Migration of Organophosphorus Flame Retardant DOPO in Plastic Polymers by HPLC-MS/MS and Its Migration Regularity
- 分析测试学报 2019年38卷第3期页码：277-282
- 作者机构：
  
  广东出入境检验检疫局技术中心
- 作者简介：
- 基金信息：
  
  国家重点研发计划（2016YFF0203705）;广东检验检疫局科研项目（2018GDK22）
- DOI：doi：10.3969/j.issn.1004-4957.2019.03.003
  中图分类号：
- 纸质出版：2019
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林春梅, 刘莹峰, 张子豪, 李全忠, 李丹, 翟翠萍, 肖前, 郑建国. 高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究[J]. 分析测试学报, 2019,38(3):277-282.

林春梅, 刘莹峰, 张子豪, 李全忠, 李丹, 翟翠萍, 肖前, 郑建国. Study on Analysis of Migration of Organophosphorus Flame Retardant DOPO in Plastic Polymers by HPLC-MS/MS and Its Migration Regularity[J]. 2019, 38(3): 277-282.
林春梅, 刘莹峰, 张子豪, 李全忠, 李丹, 翟翠萍, 肖前, 郑建国. 高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究[J]. 分析测试学报, 2019,38(3):277-282. DOI： doi：10.3969/j.issn.1004-4957.2019.03.003.

林春梅, 刘莹峰, 张子豪, 李全忠, 李丹, 翟翠萍, 肖前, 郑建国. Study on Analysis of Migration of Organophosphorus Flame Retardant DOPO in Plastic Polymers by HPLC-MS/MS and Its Migration Regularity[J]. 2019, 38(3): 277-282. DOI： doi：10.3969/j.issn.1004-4957.2019.03.003.

摘要

采用高效液相色谱-串联质谱（HPLC-MS/MS）技术建立了塑料聚合物中9

10-二氢-9-氧-10-磷杂菲-10-氧化物（DOPO）迁移量的测定方法，并对不同浸泡模拟物、不同温度和时间下DOPO的迁移规律进行研究。样品采用欧盟（EU）2017/752法规中的食品模拟物浸泡。水基模拟物直接过滤，橄榄油模拟物用含38%甲醇的乙腈溶液萃取后，经C18色谱柱分离，以甲醇-2 mmol/L醋酸铵水溶液（含0.1%甲酸）为流动相，采用多反应监测模式进行检测。水基模拟物（3%乙酸、10%乙醇、50%乙醇）中DOPO的定量下限为0.10 ng/mL，橄榄油模拟物中的定量下限为1.0 ng/g。样品加标回收率为85.3%~110%，相对标准偏差（RSD，n=6）不大于7.3%。该方法快速简便、灵敏度高、准确性好，适用于塑料聚合物中DOPO迁移量的测定。

Abstract

A method of high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was established for the determination of migration of 9

10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide（DOPO）in plastic polymers.The migration regularity of the analyte in different simulants

temperatures and times were studied.Samples were soaked with the food simulants according to（EU）2017/752.The water based simulated sample was directly filtered

and the olive oil simulated sample was extracted with acetonitrile solution containing 38% methanol.The samples were separated on a C18 column with methanol-2 mmol/L ammonium acetate containing 0.1% formic acid as mobile phases

and analyzed under multiple reaction monitoring mode.The quantitation limits of the method for water based simulant（3% acetic acid

10% alcohol

50% alcohol）and olive oil simulant were 0.10 ng/mL and 1.0 ng/g

respectively.The spiked recoveries ranged from 85.3% to 110% with relative standard deviations（RSD）not more than 7.3%.This method was rapid

precise and convenient

and was appropriate for the determination of DOPO migration in plastic polymers.

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