Identification and quantification of polyethylene glycol types in polyethylene glycol methyl ether and polyethylene glycol vinyl ether.
Identification and quantification of polyethylene glycol types in polyethylene glycol methyl ether and polyethylene glycol vinyl ether.
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DOI：
10.1016/j.chroma.2009.08.024
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发表时间：
2009-10
期刊：
影响因子：
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通讯作者：
B. N. Barman;Donald H. Champion;Stephen L. Sjoberg
中科院分区：
文献类型：
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作者：
B. N. Barman;Donald H. Champion;Stephen L. Sjoberg
采用反相高效液相色谱-蒸发光散射检测法，对聚乙二醇单功能聚乙二醇甲醚(M-PEG)和聚乙二醇乙烯基醚(V-PEG)中的杂质进行了定量测定。除了优化聚乙二醇峰和单官能团聚乙二醇峰之间的分辨率外，主要的焦点是确定不同分子量的M-聚乙二醇和V-聚乙二醇中的聚乙二醇组分的相对分子质量。后者是通过在几种情况下检查单官能团聚乙二醇组分和聚乙二醇组分的LC-MS质谱图，并将峰保留时间与所有M-聚乙二醇组分和V-聚乙二醇组分的可用的聚乙二醇组分标准的峰保留时间相匹配来实现的。这些信息有助于选择适当的聚乙二醇酯标准来确定每种样品类型中的聚乙二醇酯含量。还比较了不同聚乙二醇标准的ELSD响应因子。研究发现，相对分子质量从1000Da到8000Da的聚乙二醇酯标准品的响应度在10%以内。然而，低相对分子质量的聚乙二醇，如聚乙二醇400，与其较高相对分子质量的对应物相比，提供的响应大约少30%。
Quantitative determination of polyethylene glycol (PEG) impurities in two monofunctional polyglycol types, PEG methyl ether (M-PEG) and PEG vinyl ether (V-PEG), has been carried out by reversed-phase liquid chromatography with evaporative light scattering detection (ELSD). In addition to optimizing the resolution between PEG and monofunctional PEG peaks, the major focus has been to determine the molecular weights of PEG impurities in M-PEG and V-PEG of diverse molecular weights. The latter is achieved by examining liquid chromatography–mass spectrometry (LC–MS) mass spectra of both monofunctional PEG and PEG in several cases, and matching peak retention times with those of available PEG standards for all M-PEG and V-PEG sample types. This information is helpful in selecting the appropriate PEG standard to determine PEG content in each sample type. ELSD response factors for various PEG standards have also been compared. It has been found that PEG standards with molecular weights from 1000Da to 8000Da show responses that are within 10% of each other. However, a low molecular weight PEG such as PEG 400, provides approximately 30% less response compared to its higher molecular weight counterparts.