顶空-气相色谱法同时检测一次性使用无菌医疗器械产品中环氧乙烷和2-氯乙醇残留量的效果

The Effect of Gas Chromatographic Headspace Analysis on Simultaneous Detection of Residual Amounts of Ethylene Oxide and 2-Chloroethanol in Disposable Sterile Medical Device Products

目的探讨顶空-气相色谱法同时检测环氧乙烷(EO)灭菌的一次性使用无菌医疗器械产品中EO和2-氯乙醇(ECH)残留量的效果,并分析EO灭菌的典型一次性使用无菌医疗器械产品中EO和ECH的残留量。方法选用水作为浸提介质,基于不同条件色谱峰面积的变化确定最佳平衡温度为80℃、平衡时间为30 min、浸提比例为0.5 g/ml。分析顶空-气相色谱法检测的专属性、线性关系及EO和ECH的检出限、定量限,并验证该方法的精密度、回收率。采用顶空-气相色谱法检测典型一次性使用无菌医疗器械产品中EO和ECH的残留量。结果顶空-气相色谱法的专属性强;EO在浓度0.25~20.00μg/ml范围内线性关系良好,ECH在浓度2.50~200.00μg/ml范围内线性关系良好;EO的检出限为0.03μg/ml、定量限为0.08μg/ml,ECH的检出限为0.50μg/ml、定量限为1.50μg/ml;EO和ECH的精密度均良好,满足检测要求;EO和ECH在2种空白基质不同添加水平的平均回收率均满足检测要求;典型产品中共2个样品检出EO,其中一次性使用聚氯乙烯输液器中EO含量为0.22μg/g,医用棉垫中EO含量为2.60μg/g,所有产品均未检出ECH。结论通过最佳平衡温度、平衡时间、浸提比例建立的顶空-气相色谱法可科学有效地评价EO灭菌的一次性使用无菌医疗器械产品中EO和ECH的残留风险,具有操作简单、专属性强、定量准确、重现性好的特点,可作为一次性使用无菌医疗器械产品现行标准的有益补充。

Objective To investigate the effectiveness of gas chromatographic headspace analysis in simultaneously detecting residual levels of ethylene oxide(EO)and 2-chloroethanol(ECH)in disposable sterile medical device products sterilized with ethylene oxide(EO),and to analyze the residual levels of EO and ECH in typical disposable sterile medical device products sterilized with EO.Methods With the selection of water as the extraction medium,the changes in chromatographic peak areas with different conditions were investigated.With the optimal equilibrium temperature of 80℃,equilibrium time of 30 min and extraction ratio of 0.5 g/ml determined,the specificities and linear relationships of headspace-gas chromatography detection as well as the detection limits and quantitation limits of EO and ECH were analyzed.In addition,the precisions and recovery rates of the method were verified.Finally,this method was used to detect the residual levels of EO and ECH in typical disposable sterile medical device products.Results The gas chromatographic headspace analysis had strong specificity;For EO,the linear relationship was good within the concentration range of 0.25~20.00μg/ml,and for ECH,the linear relationship was good within the concentration range of 2.50~200.00μg/ml;The detection limit for EO was 0.03μg/ml,the quantification limit was 0.08μg/ml,and the detection limit for ECH was 0.50μg/ml,the quantification limit was 1.50μg/ml;The precisions of EO and ECH were good and met the testing requirements;The average recoveries of EO and ECH in two blank substrates with different addition levels met the detection requirements.Two typical product samples were tested for EO,with an EO content of 0.22μg/g in disposable PVC infusion sets and 2.60μg/g in medical cotton pads.In addition,no ECH was detected in any of the products.Conclusions The headspace gas chromatography method established through optimal equilibrium temperature,equilibrium time,and extraction ratio can scientifically and effectively evaluate the residual risk of EO and ECH in disposable sterile medical device products sterilized with EO.With its simple operation,strong specificity,accurate quantification,and good reproducibility,it can serve as a useful supplement to the current standards for disposable sterile medical devices.