| 基于SPME/GC × GC－QTOF MS法测定回收PET中的挥发性有机物 |
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| 基金项目:国家重点研发计划（2018YFC1603204，2018YFC1603200） |
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| 中文摘要:建立了顶空-固相微萃取（HS-SPME）结合全二维气相色谱－串联四极杆飞行时间高分辨质谱（GC × GC－QTOF MS）测定回收聚对苯二甲酸乙二醇酯（rPET）中挥发性有机物的方法。比较了不同固相微萃取纤维头、萃取温度、顶空平衡时间、调制周期和升温速率对测定效果的影响，用NIST谱库结合色谱保留指数对物质进行定性，并对高频检出物质进行半定量。结果表明，最佳检测条件为：80 μm DVB/C-WR/PDMS萃取纤维头、萃取温度110 ℃、平衡时间30 min、二维调制周期4 s、色谱升温速率8 ℃/min。9个回收PET样品中共检出209种挥发性有机物，包括苯系物、烷烃类、醇类、醛酮类、酯类、烯烃类、萘类、羧酸类和酚类等。高频物质的最高含量为2.13 mg/kg（十四烷），未发现浓度极高的误用物质。该研究为回收PET中的挥发性有机物调查提供了科学和可靠的方法依据，并为回收PET的利用和安全评估提供了基础数据。 |
| 中文关键词:回收PET 全二维气相色谱－串联四极杆飞行时间高分辨质谱 挥发性有机物 方法优化 |
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| Determination of Volatile Organic Compounds in Recycled Polyethylene Terephthalate by SPME/GC × GC－QTOF MS |
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| Abstract:Polyethylene terephthalate（PET） is an excellent material for recycling due to its low diffusivity and low sorption features．The ideal recycling is to use the recycled PET（rPET） material for the initial intended use．There are some intentionally added and non-intentionally added risk substances in rPET．There will be some safety risks if these substances migrate into food．Due to insufficient data on rPET pollutants for safety assessment，rPET cannot be used in food contact materials in China．In this study，a method was established for the analysis of volatile organic compounds（VOCs） in rPET using comprehensive two-dimensional gas chromatography－quadrupole time-of-flight mass spectrometry（GC × GC－QTOF MS） combined with headspace solid phase microextraction（HS-SPME）．Influences of different SPME fibers（PDMS，DVB/PDMS and DVB/C-WR/PDMS），extraction temperatures（50，70，90，110，130，150 ℃），headspace equilibrium times（15，30，60 min），modulation periods（2，4，6 s） and heating rates of oven（3，5，8，10 ℃/min） on the determination effect were compared．The VOCs were identified with NIST library combined with Kovats indexes．The content of high-frequency compounds was determined by semi-quantification．The best HS-SPME and instrument conditions were as follows：SPME fiber：80 μm DVB/C-WR/PDMS，extraction temperature：110 ℃，equilibrium time：30 min，modulation period：4 s，and heating rate of oven：8 ℃/min. 209 volatile organic compounds were determined in 9 rPET samples，including aromatic compounds，alkanes，alcohols，aldehydes，ketones，esters，olefins，naphthalene，carboxylic acids and phenols．Aromatic compounds could be derived from the degradation of rPET in different environments．Terpene may come from the residue of flavor substances in early PET bottle drinks．Among the 9 rPET samples，the substances with detection frequency greater than 5 were d-limonene，γ-terpinene，5-methyl-1-undecene，tetradecane，naphthalene，1-methyl-naphthalene，1-ethylidene-1h-indene，2-dodecanol，2-decanone and 2，4-di-tert-butylphenol．D-Limonene is a common pollutant in rPET，which comes from the contact between original PET bottle and beverage．2，4-di-tert-butylphenol may be the degradation product of antioxidant 168，and remaining in rPET．The highest content of high-frequency compounds was 2.13 mg/kg（tetradecane）．No misused compound with extremely high concentration was found．This research provided not only a scientific and reliable methodological basis for the investigation of VOCs in rPET，but also the basic data for utilization and safety assessment of rPET. |
| Key Words:recycled polyethylene terephthalate（rPET） comprehensive two-dimensional gas chromatography－quadrupole time of flight mass spectrometry volatile organic compounds method optimization |
| 引用本文：叶智康，曾莹，林勤保 ，吴学峰，郝天英，董犇，李丹，钟怀宁.基于SPME/GC × GC－QTOF MS法测定回收PET中的挥发性有机物[J].分析测试学报,2021,40(11):1596-1603. |
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