Gayan Premaratne, Andrew McAdoo, Jingzhi Tian, Abu Rustum
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引用次数: 0
摘要
本文建立了一种顶空气相色谱法（HSGC）测定散装聚乙二醇（PEG）中环氧乙烷（EO）和1,4-二恶烷（Dioxane）的新方法。PEG样品溶解在二甲亚砜中，在90°C的顶空烘箱中加热10分钟，然后注入GC系统进行分析。分析物在Agilent DB-624色谱柱（60 m × 0.53 mm直径，膜厚3.00 μm）上通过36至240°C的热梯度洗脱分离。载气为氦，探测器为火焰电离探测器。新HSGC方法的总运行时间约为18 min。在新HSGC方法中，其他常见的残留溶剂如甲醇（MeOH）、甲酸甲酯（MF）和乙酰醛（Acetal）也能与EO和二氧六环峰充分分离。在USP专论和EP专论规定的HSGC方法中，EO与MF共洗脱。新的HSGC方法根据现行ICH/VICH指南成功验证，具有特异性、线性性、准确性、精密度、鲁棒性和敏感性。HSGC方法快速，质量控制友好，适用于QC实验室散装peg中EO和二氧六环的常规分析。
A New Headspace Gas Chromatography Method for Determination of Ethylene Oxide and Dioxane in Polyethylene Glycols.
In this paper, a new headspace gas chromatography (HSGC) method has been developed for the determination of ethylene oxide (EO) and 1,4-Dioxane (Dioxane) in bulk lots of polyethylene glycols (PEG). PEG samples are dissolved in dimethyl sulfoxide, heated in a headspace oven maintained at 90°C for 10 min and then injected into the GC system for analysis. Analytes are separated through a thermal gradient elution from 36 to 240°C on an Agilent DB-624 column (60 m × 0.53 mm diameter, film thickness 3.00 μm). The carrier gas is helium and detector is flame ionization detector. Total run time of the new HSGC method is about 18 min. In the new HSGC method, other common residual solvents present in PEGs such as methanol (MeOH), methyl formate (MF) and acetyl aldehyde (Acetal) are also sufficiently separated from EO and Dioxane peaks. In the HSGC methods prescribed in USP monograph <228> and EP monograph <2.4.25>, EO co-elutes with MF. The new HSGC method was successfully validated according to current ICH/VICH guidelines and was found to be specific, linear, accurate, precise, robust and sensitive. This HSGC method is fast and quality control (QC) friendly and suitable for routine analysis for the determination of EO and Dioxane in bulk batches of PEGs in QC laboratories.
期刊介绍：
The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.
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