响应面优化光度法测定口罩中环氧乙烷含量

Determination of ethylene oxide in masks by spectrophotometry optimized via response surface methodology

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。

It is an important means to ensure the quality and safety of masks by monitoring the ethylene oxide(EO)residue in masks.In this work,an acetylacetone spectrophotometric method for the determination of EO residue in masks was established by response surface methodology(RSM).The optimal experimental condition was obtained by investigating the effects of ultrasonic extraction time,hydrochloric acid concentration and color reaction time.It was found that the interaction of the three factors on the average recoveries of the spiked samples was significant.The optimal average recovery of the spiked sample was at 101.09%,when the experimental conditions were selected with the ultrasonic extraction time at 58.9 min,the hydrochloric acid concentration at 0.24 moL·L^(-1)and the color reaction time at 27.78 min.The RSM results were further verified by single factor method and showed in good agreement.The linearities were obtained ranging from 0μg·g^(-1)to 50.00μg·g^(-1)with correlation coefficients(R2)higher than 0.995 for the target EO.The recoveries were between 98.2%~101.2%at the spiked levels with the relative standard deviations(RSDs)in the range of 1.5%~4.2%(intra day)and 1.8%~4.7%(7 days inter day),respectively.The limit of detection(LOD)and the limit of quantification(LOQ)were at 0.026μg·g^(-1)and 0.087μg·g^(-1),respectively.Compared with literature reported methods,the present work showed advantages of simple operation with low LOD.The residual amount of EO in 8 kinds of masks with different materials and storage time was determined.The results showed that the residual amount of EO in commercially available medical surgical masks was at 1.52μg·g-1,which met the requirements of the national standard.The residual amount of EO in the used mask samples decreased with storage time.This method can be used for rapid screening and confirmatory analysis of ethylene oxide residues in masks.