柱前衍生-反相高效液相色谱法测定人血白蛋白中辛酸钠含量

Detection of Sodium Caprylate in Human Serum Albumin by Precolumn Derivation Reversed Phase High Performance Liquid Chromatography

建立了柱前衍生-反相高效液相色谱法测定人血白蛋白中辛酸钠含量的方法。用正己烷萃取人血白蛋白中的辛酸钠,与ω-溴苯乙酮和18-冠-6醚在50℃反应30min,然后用甲醇-水(75∶25,V/V)于Nova-ParkC18柱(150mm×3.9mm,4μm)上分离,在262nm检测衍生物,流速为1.0mL/min,庚酸为内标。辛酸和庚酸的萃取率可分别达到98.2%和97.9%,RSD小于0.9%。方法的线性范围为9.00×10-4～1.44×10-2mol/L(r=0.9995),平均加样回收率为99.7%,RSD≤0.9%。本方法准确、重现性好,可用于人血白蛋白中辛酸钠含量的测定。

A method was developed for the determination of sodium caprylate in human serum albumin by reversed phase high performance liquid chromatography （ RP-HPLC） after pre-column derivatization. The caprylic acid,extracted from human serum albumin by hexane,was treated with ω-bromoacetophenone and 18-crown-6 for 30 min at 50 ℃,and analyzed on a Nova-Park C18（ 150 mm × 3. 9 mm,4 μm） column with methanol-water（ 75∶25,V/V） as the mobile phase. The internal standard was enanthic acid,the flow rate was 1. 0 mL/min and the detection wavelength was 262 nm. The extraction yield of caprylic acid was 97. 9% and that of enanthic acid was 98. 2% . The linear range of sodium caprylate was 9. 00 × 10-4-1. 44 × 10-2 mol/L （ r =0. 9995） . The average recovery of caprylic acid was 99. 7%,RSD was less than 0. 9%. The present method is reliable and relatively simple and can be used for the determination of sodium caprylate in human serum albumin.