摘要
建立了血液透析器中可沥滤物的气相色谱-三重四极杆质谱(GC-MS)分析方法。以丙酮为浸提溶剂,超声30 min浸提血液透析器透析膜中的可沥滤物,浸提液过滤后GC-MS法定性,外标法定量。2种主要可沥滤物鉴定为1,3-二叔丁基苯和2,4-二叔丁基苯酚,分别在0.80~12.80 mg/L和0.88~14.88 mg/L范围内线性关系良好,相关系数(r)分别为0.9992和0.9950。3个加标水平下,1,3-二叔丁基苯的加标回收率为93.8%~105.8%,相对标准偏差(RSD)为0.80%~1.4%,检出限(LOD)为0.026μg/g,定量限(LOQ)为0.087μg/g;2,4-二叔丁基苯酚的加标回收率为95.8%~107.3%, RSD为0.65%~1.0%, LOD为0.826μg/g,LOQ为2.76μg/g。该方法可为完善血液透析器的质量控制和监管提供新的技术支持。
A gas chromatography-triple quadrupole mass spectrometry(GC-MS)method was established for the determination of leachable substance in haemodialysers.Using acetone as the leaching solvent,the leachable substance in the dialysis membrane of the haemodialyser was leached by ultrasonic extraction for 30 min.The extract was identified by GC-MS and quantified by external standard method.The two main leachable substance were identified as 1,3-di-tert-butylbenzene and 2,4-di-tert-butylphenol,which had linear relationships in the ranges of 0.80-12.80 mg/L and 0.88-14.88 mg/L,with the correlation coefficients(r)of 0.9992 and 0.9950,respectively.The recovery rates of 1,3-di-tert-butylbenzene were 93.8%-105.8%at three spiked levels,and the relative standard deviations(RSDs)were 0.80%-1.4%,with the limit of detection(LOD)of 0.026μg/g and the limit of quantification(LOQ)of 0.087μg/g.The recovery rates of 2,4-di-tert-butylphenol was 95.8%-107.3%,and the RSDs were 0.65%-1.0%,with the LOD of 0.826μg/g and the LOQ of 2.76μg/g.This method could provide new technical support for improving the quality control and supervision of haemodialysers.
作者
刘子琪
陈卓颖
刘璟
韩倩倩
付步芳
LIU Ziqi;CHEN Zhuoying;LIU Jing;HAN Qianqian;FU Bufang(National Institutes for Food and Drug Control,Beijing 102629,China;School of Pharmacy,China Pharmaceutical University,Nanjing 211198,China;School of Materials Science and Engineering,South China University of Technology,Guangzhou 510641,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2023年第6期730-736,共7页
Chinese Journal of Analysis Laboratory
基金
国家重点研发计划(专项)(2017YFC1105000)资助。
关键词
血液透析器
可沥滤物
气相色谱-三重四极杆质谱
超声浸提
haemodialyser
leachable substance
gas chromatography-triple quadrupole mass spectrometry
ul-trasonic extraction
