气相色谱法测定依达拉奉中有机溶剂的残留量

Determination of Organic Acetate Solvents in Edaravone by Gas Chromatography

建立了依达拉奉原料药中乙醇、乙酸乙酯残留量的测定方法。采用Rtx-5毛细管柱,程序升温法,FID检测器,以外标法进行测定残留溶剂的含量。乙醇、乙酸乙酯在所考察的浓度范围内线性关系良好,平均回收率分别为98.41%(RSD=3.2%)、100.4%(RSD=4.4%);检测限分别为3.09 ng、2.88 ng,精密度、重复性、稳定性的RSD值均小于5%;乙醇,乙酸乙酯残留含量均符合药典规定。该方法简便、快速、灵敏及重现性好,适用于依达拉奉原料药中有机溶剂残留量的测定。

A method for determination of ethanol and ethyl acetate residual in edaravone was established. A Rtx-5capillary column, a temperature program and the flame ionization detector were used for the separation and quantitativeanalysis. A capillary gas chromatography method for determining residual organic solvents was established by externalstandard method. Ethyl alcohol and ethyl acetate had good linear relationship in the concentration range investigated. Therecoveries were 98.41% and 100.4% , RSD were 3.2% and 4. 4% , respectively, the limit of detection were 3.09 ngand 2. 88 ng, respectively, both RSD of precision, reproducibility and value stability were less than 5%, the residualsolvent amount of ethanol and ethyl acetated in line with the pharmacopoeia. The method is simple, fast, sensitive andwith good reproducibility. It can be used as a method for the determination of edaravone residual organic solvents.