论文部分内容阅读
目的建立依达拉奉中甲醇、乙醇、乙腈、四氢呋喃和乙酰乙酸乙酯5种残留有机溶剂的分离测定方法。方法采用GC法测定,以乙酸乙酯为内标,二甲基亚砜为溶媒,毛细管柱为Thermo TG-624气相色谱柱,FID检测器,载气为氮气,流速为3.0 mL·min-1,采用程序升温,初始柱温为50℃,保持2 min,以10℃·min-1升至180℃,保持5 min,进样口温度为200℃,检测器温度为210℃,用内标法计算残留溶剂的含量。结果 5种残留溶剂和内标物峰面积的比值在测定的浓度范围内,专属性好,具有良好的线性关系,精密度RSD≤1.6%,平均回收率为99.5%~100.7%(n=9)。结论所用方法简单、准确、灵敏,适用于依达拉奉中甲醇、乙醇、乙腈、四氢呋喃和乙酰乙酸乙酯5种残留溶剂的同时测定。
OBJECTIVE To establish a method for the separation and determination of five residues of edaravone in methanol, ethanol, acetonitrile, tetrahydrofuran and ethyl acetoacetate. Methods The GC method was used. The internal standard was ethyl acetate and dimethylsulfoxide was used as the solvent. The capillary column was Thermo TG-624 gas chromatography column and FID detector. The carrier gas was nitrogen and the flow rate was 3.0 mL · min -1 , The temperature was programmed, the initial column temperature was 50 ℃, holding 2 min, 10 ℃ · min-1 rose to 180 ℃ for 5 min, the inlet temperature was 200 ℃, the detector temperature was 210 ℃, with internal standard Method to calculate the residual solvent content. Results The ratio of the peak area of the five kinds of residual solvents and the internal standard was within the range of the measured concentration, with good specificity and good linearity. The precision RSD was less than or equal to 1.6% and the average recovery was 99.5% ~ 100.7% (n = 9 ). Conclusion The method is simple, accurate and sensitive and suitable for the simultaneous determination of 5 residues of edaravone in methanol, ethanol, acetonitrile, tetrahydrofuran and ethyl acetoacetate.