氢醌-双(β-羟乙基)醚工业品中相关杂质的气相色谱-飞行时间质谱定性研究

建立了气相色谱 -飞行时间质谱 ( GC-TOFMS)法测定聚氨酯扩链剂氢醌 -双 ( β-羟乙基 )醚 ( HQEE)工业品中相关杂质的方法。以 5 0 mg HQEE溶解于约 5 0 m L异丙醇中 ,选用 HP-5毛细管柱 ( 3 0 m× 0 .2 5 mm× 0 .2 5μm)进行分离并对其中所含相关杂质进行了定性研究 ,通过色谱保留值和质谱图的信息推断出HQEE样品中主要杂质。结果表明 :样品中三个主要杂质均可被准确定性为 HQEE的同系物 ,相对分子质量分别为 1 5 4、2 42和 2 86。根据合成工艺路线推测出杂质的结构。考察了样品合成过程中环氧乙烷的用量。该方法可及时解决 HQEE产品在合成工艺中出现的问题 ,有效控制并提高产品的质量

Identification of the Impurities in Hydroquinone Bis(2-hydroxyethyl)ether Industrial Products by Gas Chromatography-Time of Flight Mass Spectrometry

A method for identification of the interrelated impurities in some kind of chain extender for polyurethane, hydroquinone bis(2-hydroxyethyl)ether (HQEE) industrial products by gas chromatography-time of flight mass spectrometry(GC-TOFMS) was developed. 50mg HQEE samples was dissolved in 50mL iso-propyl alcohol, and injected into HP-5 capillary column (30m×0.25mm×0.25μm). Three peaks from the total ion current chromatogram of HQEE samples were qualitatively confirmed by comparing with the retention time and MS spectrum of HQEE standard. The results showed that three main impurities were accurately identified to be homologeous compounds with the relative molecular mass of 154, 242 and 286, respectively. Under selected GC/TOFMS conditions, all components were fully separated. According to the synthesis process, the structures of the three impurities were proposed. The practical amount of ethylene oxide in the sample synthesis was in-vestigated. The method will help to effectively control and improve product quality in HQEE synthesis.