气相色谱法测定人血白蛋白半成品中辛酸钠含量

Determination of Sodium Caprilate in the Human Albumin Semi-finished Product by Gas Chromatography

目的:建立气相色谱法测定人血白蛋白半成品中辛酸钠的含量。方法:色谱条件:色谱柱KB-INNOWAX(30 m×0.32mm×0.5μm);气化室温度250℃;柱温190℃;检测器温度250℃;载气为氮气,柱流速3.0 m L·min^(-1);氢气流速40 m L·min^(-1);分流比10∶1,乙酸乙酯为萃取剂(溶剂)。进行了专属性、重复性、线性、溶液稳定性、准确度、定量限方法学验证。结果:该气相色谱法辛酸峰拖尾因子1.10,理论板数为21251,与相邻峰分离度为5.1且未受其他峰干扰。重复性RSD为0.74%;线性范围在157~785μg·m L^(-1);溶液在24 h内稳定,峰面积RSD为1.01%;平均回收率及RSD分别为96.72%±0.93%、0.96%,定量限为5.23μg。结论:本文建立的气相色谱法测定人血白蛋白半成品中辛酸钠的含量,操作简便、准确。

Objective： To establish a method for determination of Sodium Caprilate in the Human Albumin semi-finished product by gas chromatography. Methods： The chromatographic conditions were as follows ： KB INNOWAX column （ 30 m x 0. 32mmX0.5μm） ; the gasification room temperature as 250 ℃ ; the column temperature as 190 ℃; the detector temperature was 250 ℃, N2 as the carrier gas and column flow rate as 3.0 mL · min-1 ; hydrogen flow rate was 40 mL · min-1 ; the split ratio as 10：1 ; and ethyl acetate as the extraction solvent. The specificity, repeatability, linearity range, solution stability, accuracy and limit of quantification of this method were validated. Results： The tailing factor of Capri!ate peak was 1. 10, its theoretical plate number was 21251, and the resolu- tion of Caprilate peak with adjacent peaks was 5. 1. The RSD of repeatability was 0. 74%, the linearity range was 157-785 μg · mL-1 , and the RSD of peak area for the solution stability within 24 hours was 1.01%. The average recovery was 96. 72% ±0.93% with RSD as 0. 96%. The LOQ was 5.23 μg. Conclusion： The method is simple, and reliable which can be used for determination of Sodium Caprilate in the Human Albumin semi-finished product.