Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively...Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively inert, causing no irritation and allergies. Poly(ethylene oxide)(PEO) hydrogels were prepared using pentaerythritol tetra-acrylate(PETRA) as UV crosslinking agent. A simple, accurate, and robust quantitation method was developed based on gas chromatographic techniques(GC), which is suitable for routine analysis of residual PETRA monomers in these hydrogels. Unreacted PETRA was initially identified using gas chromatography–mass spectrometry(GC–MS). The quantitation of analyte was performed and validated using gas chromatography equipped with a flame ionization detector(GC–FID). A linear relationship was obtained over the range of 0.0002%–0.0450%(m/m) with a correlation coefficient(r2)greater than 0.99. The recovery( 4 90%), intra-day precision(%RSD o 0.67), inter-day precision(%RSD o2.5%), and robustness(%RSD o1.62%) of the method were within the acceptable values. The limit of detection(LOD) and limit of quantitation(LOQ) were 0.0001%(m/m) and 0.0002%(m/m), respectively.This assay provides a simple and quick way of screening for residual acrylate monomer in hydrogels.展开更多
文摘Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively inert, causing no irritation and allergies. Poly(ethylene oxide)(PEO) hydrogels were prepared using pentaerythritol tetra-acrylate(PETRA) as UV crosslinking agent. A simple, accurate, and robust quantitation method was developed based on gas chromatographic techniques(GC), which is suitable for routine analysis of residual PETRA monomers in these hydrogels. Unreacted PETRA was initially identified using gas chromatography–mass spectrometry(GC–MS). The quantitation of analyte was performed and validated using gas chromatography equipped with a flame ionization detector(GC–FID). A linear relationship was obtained over the range of 0.0002%–0.0450%(m/m) with a correlation coefficient(r2)greater than 0.99. The recovery( 4 90%), intra-day precision(%RSD o 0.67), inter-day precision(%RSD o2.5%), and robustness(%RSD o1.62%) of the method were within the acceptable values. The limit of detection(LOD) and limit of quantitation(LOQ) were 0.0001%(m/m) and 0.0002%(m/m), respectively.This assay provides a simple and quick way of screening for residual acrylate monomer in hydrogels.
文摘对口罩中环氧乙烷残留量进行监测是确保口罩质量安全的重要手段。本文采用响应面法(Response Surface Methodology,RSM)建立了口罩中环氧乙烷含量定量检测的乙酰丙酮光度法。通过考察超声提取时间、盐酸浓度和显色反应时间优化了实验条件。发现这三个因素对加标样品平均回收率的影响交互作用明显;超声提取时间58.9 min、盐酸浓度0.24 moL·L^(-1)和显色反应时间27.78 min时,加标样品平均回收率可达最佳值(101.09%)。通过单因素法进行验证,所建立的检测方法检出限(limit of detection,LOD)和定量限(limit of quantification,LOQ)分别为0.026μg·g^(-1)和0.087μg·g^(-1)。浓度为0~50.00μg·g^(-1)范围内线性相关系数(R^(2))大于0.995,平均加标回收率为98.2%~101.2%,日内精密度为1.5%~4.2%,日间精密度(7天)为1.8%~4.7%。与文献方法相比具有操作简单、检出限低等优点。对8种不同材质和放置时间的实际口罩样品进行检测。发现市售医用外科口罩样品中环氧乙烷的残留量为1.52μg·g^(-1),符合国标要求。使用后的口罩样品中环氧乙烷的残留量随着时间延长残留量下降。本文所建立的方法可用于口罩中环氧乙烷残留量的快速筛查和确证分析。
