液相色谱-高分辨质谱法定性定量检测血液透析器中3种未知可沥滤物  

Qualitative and Quantitative Detection of 3 Unknown Leachable Substances in Hemodialyzers by Liquid Chromatography-High Resolution Mass Spectrometry

作　　者：刘子琪 黄元礼[1] 付步芳[1] LIU Ziqi;HUANG Yuanli;FU Bufang(National Institutes for Food and Drug Control,Beijing 102629,China;Shandong Lab of Advanced Biomaterials and Medical Devices in Weihai,Weihai 264209,China)

机构地区：[1]中国食品药品检定研究院,北京102629 [2]威海先进医用材料与高端医疗器械山东省实验室,威海264209

出　　处：《理化检验（化学分册）》2024年第12期1209-1215,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重点研发计划(专项)(2017YFC1105000)。

摘　　要：参考血液透析器说明书以及GB/T 14232.1—2020,分别采用水和乙醇-水混合溶液浸提血液透析器中可沥滤物,液相色谱-高分辨质谱法采集浸提液中未知可沥滤物的色谱、质谱信息,并以二甲基乙酰胺为例介绍了定性流程,外标法测定了可沥滤物的含量。结果显示,在1.7,2.1,2.5 min附近发现3种可沥滤物,经质谱解析和对照品比对,分别确定为2-吡咯烷酮、二甲基乙酰胺和N-甲基吡咯烷酮。3种可沥滤物的质量浓度分别在0.089 6~4.48 mg·L^(-1),0.469 5~18.78 mg·L^(-1)和0.102 6~5.130 mg·L^(-1)内与其对应的定量离子的峰面积呈线性关系,检出限(3S/N)分别为0.005 1,0.009 9,0.010 5μg·g-1。方法用于28个血液透析器的分析,乙醇-水浸提液中3种可沥滤物的溶出量高于水浸提液中的,最大溶出量分别为376.7,2 668.4,517.8μg。Referring to the hemodialyzer instructions and GB/T 14232.1—2020,water and ethanol-water mixed solution were used to extract leachable substances from the hemodialyzer.The chromatography and mass spectrometry information of unknown leachable substances in the extract was collected by liquid chromatography-high resolution mass spectrometry.The qualitative process was introduced using dimethylacetamide as an example,and the content of leachable substances was determined by external standard method.It was shown that 3 leachable substances were found around 1.7,2.1,2.5 min,which were determined to be 2-pyrrolidone,dimethylacetamide,and N-methylpyrrolidone after mass spectrometry analysis and comparison with reference substances.Linear relationships between values of the mass concentration of 3 leachable substances and the corresponding peak area of quantitative ions were kept in the ranges of 0.0896-4.48 mg·L^(-1),0.4695-18.78 mg·L^(-1),and 0.1026-5.130 mg·L^(-1),with detection limits(3S/N)of 0.0051,0.0099,0.0105μg·g-1.The method was used for the analysis of 28 hemodialyzers,and the leaching amounts of 3 leachable substances in ethanol-water extract were higher than those in water extract,with the maximum leaching amounts of 376.7,2668.4,517.8μg,respectively.

关 键 词：血液透析器 液相色谱-高分辨质谱联用法 可沥滤物 

分 类 号：O657.63[理学—分析化学] O657.7[理学—化学]