毛细管气相色谱法测定氯高铁血红素原料药中的冰醋酸残留量

目的：测定氯高铁血红素原料药中的冰醋酸残留量。方法：采用毛细管气相色谱法。色谱柱为PEG-20M的石英毛细管柱,柱温为160℃,氢火焰离子化检测器,温度为250℃,载气为氮气,助燃气为氢气和空气,以蒸馏水为溶剂制备溶液直接进样,进样量为1.0μL。结果：冰醋酸检测浓度线性范围为0.00638～0.12751mg·mL-1（r=1.0000）;低、中、高浓度平均回收率（n=9）分别为98.98%、97.76%、98.86%,RSD分别为3.19%、2.06%、1.98%;最低检测限为0.00076mg·mL-1。结论：该法可用于氯高铁血红素原料药中冰醋酸残留量的检测。

Detection of Residual Glacial Acetic Acid in Hematin Chloride Raw Materials by Capillary Gas Chromatography

OBJECTIVE：To establish the method for the determination of residual glacial acetic acid in hematin chloride raw materials.METHODS：Capillary gas chromatography was adopted.The determination was performed on PEG-20M quartz capillary column with column temperature of 160 ℃.Flame ionization detector was used and the temperature of it was 250 ℃ with nitrogen as carrier gas,and hydrogen and air as auxiliary gas using distilled water as solvent for direct-injection detection.The injection volume was 1.0 μL.RESULTS：The linear range of glacial acetic acid was 0.006 38～0.127 51 mg·mL-1（r=1.000 0）;the average recoveries were 98.98%,97.76% and 98.86% at low,middle and high concentration（n=9） with RSD of 3.19%,2.06% and 1.98%.The detection limit was 0.000 76 mg·mL-1.CONCLUSION：The method can be used to detect residual glacial acetic acid in hematin chloride raw materials.