| 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 |
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| 基金项目:国家重点研发计划（2016YFF0203705）；广东检验检疫局科研项目（2018GDK22） |
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| 中文摘要: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。 |
| 中文关键词:有机磷阻燃剂 迁移量 DOPO 高效液相色谱-串联质谱（HPLC-MS/MS） |
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| Study on Analysis of Migration of Organophosphorus Flame Retardant DOPO in Plastic Polymers by HPLC-MS/MS and Its Migration Regularity |
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| 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. |
| Key Words:plastic organophosphorus flame retardant migration DOPO high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） |
| 引用本文：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. |
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