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Fully Automated Determination of Trimellitic Anhydride in Saturated Polyester Resins Using Programmed Temperature Vaporization-Large Volume Injection-Gas Chromatography Previous Aqueous Derivatization with Triethyloxonium Tetrafluoroborate
Chromatographia ( IF 1.7 ) Pub Date : 2020-03-25 , DOI: 10.1007/s10337-020-03877-0
Stefano Dugheri , Giorgio Marrubini , Andrea Speltini , Nicola Mucci , Giovanni Cappelli , Gianluca Bartolucci , Giulio Arcangeli

Trimellitic anhydride (TMAn) is an essential starting material of the chemical manufacturing industry; it is widely used in saturated polyester resins (SPR) manufacturing to produce plasticizers for different purposes. TMAn was recently added, as a new substance of very high concern, to the candidate list by the European Chemicals Agency, since it can lead to sensitization, respiratory tract irritation and lung disease. Any substance from the list of candidates if present in manufactured products at concentrations above 0.1% (w/w) obliges the manufacturer to communicate this to customers down the supply chain and to consumers. We propose here a method that allows the fully automated determination of TMAn in SPR samples by using large volume injection (LVI), with programmed temperature vaporization (PTV) injection, in a gas chromatographic (GC) system equipped with ion trap mass spectrometer (IT) operating in tandem mass spectrometry (MS/MS). The method optimization was obtained by a chemometric model, using the experimental design. Introducing the use of short chromatographic column, triethyloxonium tetrafluoroborate (TEO) as derivatization agent and IS granted specificity, sensitivity and robustness. The detection and quantification limits for TMAn were 0.01% and 0.03% w/w, respectively. Trueness (between 94 and 98%) and precision (RSD lower than 10%, n = 6) were also assessed.

中文翻译:

使用程序升温汽化-大体积进样-气相色谱法全自动测定饱和聚酯树脂中的偏苯三酸酐

偏苯三酸酐 (TMAn) 是化学制造工业的重要原材料;广泛用于饱和聚酯树脂(SPR)制造,生产不同用途的增塑剂。TMAn 最近作为一种高度关注的新物质被欧洲化学品管理局添加到候选清单中,因为它会导致过敏、呼吸道刺激和肺部疾病。候选清单中的任何物质如果以高于 0.1% (w/w) 的浓度存在于制成品中,则制造商有义务将其传达给供应链下游的客户和消费者。我们在此提出了一种方法,该方法允许通过使用大体积进样 (LVI) 和程序升温汽化 (PTV) 进样来全自动测定 SPR 样品中的 TMAn,在配备离子阱质谱仪 (IT) 串联质谱 (MS/MS) 的气相色谱 (GC) 系统中。方法优化是通过化学计量模型获得的,使用实验设计。介绍使用短色谱柱、四氟硼酸三乙基氧鎓 (TEO) 作为衍生剂和 IS 获得特异性、灵敏度和稳健性。TMAn 的检测限和定量限分别为 0.01% 和 0.03% w/w。还评估了真实度(94% 和 98% 之间)和精密度(RSD 低于 10%,n = 6)。四氟硼酸三乙基氧鎓 (TEO) 作为衍生剂和 IS 具有特异性、敏感性和稳健性。TMAn 的检测限和定量限分别为 0.01% 和 0.03% w/w。还评估了真实度(94% 和 98% 之间)和精密度(RSD 低于 10%,n = 6)。三乙基氧鎓四氟硼酸盐 (TEO) 作为衍生剂和 IS 具有特异性、灵敏度和稳健性。TMAn 的检测限和定量限分别为 0.01% 和 0.03% w/w。还评估了真实度(94% 和 98% 之间)和精密度(RSD 低于 10%,n = 6)。
更新日期:2020-03-25
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