离子色谱法测定人血白蛋白制品中辛酸钠的含量
Determination the content of sodium caprylate in human blood albumin products by ion chromatography
严翠霞 1史芳亮 1韩春霞 2方欣欣 1郑璐侠 1邵泓1
作者信息
- 1. 上海市食品药品检验研究院国家药监局治疗类单抗质量控制重点实验室,上海 201203
- 2. 赛默飞世尔科技(中国)有限公司,上海 201203
- 折叠
摘要
目的:建立离子色谱法测定人血白蛋白制品中辛酸钠的含量.方法:样品加淋洗液[甲醇-乙腈-1.0 mmol·L-盐酸(20:42:38)]沉淀蛋白,离心取上清液,过滤后直接进样,以庚酸为内标.采用Dionex InPacTMNS1 分析柱(250 mm ×4 mm,10 μm)与 Dionex InPacTMNG1 保护柱(35 mm ×4 mm,10μm),流速1.0 mL·min-1,ASRS 300膜抑制器,化学抑制,再生液为5 mmol·L-1四丁基氢氧化钠溶液,电导检测器检测,柱温30 ℃,进样量25μL.结果:辛酸峰与内标峰间的分离度＞1.5;辛酸钠在0.38～2.52 mmol· L-1范围内线性关系良好,r=0.999 5(n=6);重复性试验的RSD为1.1％(n=6);平均加样回收率为97.4％,RSD为1.8％(n=9);定量限与检测限分别为0.19 nmol与0.09 nmol;国内外7家企业20批人血白蛋白制品中辛酸钠含量范围为0.073-0.163 mmol·g-1.结论:本研究建立的方法操作简便易行,结果准确,灵敏度高,重复性好,可用于人血白蛋白制品中辛酸钠含量的测定,为其质量控制提供方法保证.
Abstract
Objective:To establish an ion chromatography method for determination the content of sodium capry-late in human blood albumin products.Methods:The samples were precipitated with eluent,the suspension was centrifuged and filtered,the filtrate was injected to IC,and heptanoic acid was used as the internal standard.A Dionex InPacTM NS1 Analytical Column(250 mm ×4mm,10 μm)and a Dionex InPacTM NG1 Guard Column(35 mm ×4 mm,10 μm)were used,the flow rate was 1.0 mL·min-1.The conductivity detector and ASRS 300 membrane suppressor were used,and the regenerant solution was 5 mmol·L-1 tetrabutylsodium hydroxide solution;the column temperature was 30 ℃ and the injection volume was 25 μL.Results:The resolution between the peaks of sodium caprylate and the internal standard was greater than 1.5,and the linearity of concentration of sodium caprylate was good in the range of 0.38-2.52 mmol·L-1,r=0.999 5(n=6).The RSD of the repeat-ability test was 1.1％(n=6).The average recovery was 97.4％and RSD was 1.8％(n=9).The limits of quantification and detection were 0.19 nmol and 0.09 nmol,respectively.The determination results of the content of sodium octanoate in 20 batches of human blood albumin samples from 7 enterprises at home and abroad ranged from 0.073-0.163 mmol·g-1.Conclusion:The method established in this study is simple to operate,accurate in results,high in sensitivity and good in repeatability,can be used for the determination of sodium caprylate con-tent in human blood albumin products and provide a method guarantee for its quality control.
关键词
离子色谱法/内标法/人血白蛋白/辛酸钠/质量控制Key words
ion chromatography/internal standard method/sodium caprylate/human blood albumin/quality control引用本文复制引用
基金项目
上海市研发公共服务平台项目(19DZ2294600)
出版年
2024
NETL
NSTL
万方数据