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

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^(-1)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, 10μm)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。

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 InPac TM NS1 Analytical Column(250 mm×4mm,10μm)and a Dionex InPac TM NG1 Guard Column(35 mm×4 mm,10μm)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 25μL.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=0.9995(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.