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目的:建立差示扫描量热(DSC)法测定甘露六烟酯原料药的含量。方法:以铟进行仪器校正,包括温度校正和热流校正;气氛为氮气,流速20 ml·min~(-1);称样量1~3.5 mg,精确到0.01 mg;起始温度30℃,以10℃·min~(-1)速率升温至120℃,120℃保持1 min,再以2.5℃·min~(-1)速率升温至280℃。比较DSC法与HPLC法的测定结果。结果:甘露六烟酯在1.05~3.44 mg范围内,吸热量与称样量线性关系良好(r=0.999 0)。平均回收率为98.86%(RSD=1.59%,n=9)。HPLC法和DSC法测定甘露六烟酯原料药含量的结果分别为97.77%和97.80%,两值的相对平均偏差为0.015%。结论:DSC法准确度高、操作简便,可与HPLC法共同用于甘露六烟酯的含量测定。
OBJECTIVE: To establish a differential scanning calorimetry (DSC) method for the determination of the content of raw materials of nerolidin. Methods: The instrument was calibrated with indium, including temperature correction and heat flux correction. The atmosphere was nitrogen and the flow rate was 20 ml · min -1. The sample volume was 1 ~ 3.5 mg, accurate to 0.01 mg. The initial temperature was 30 ℃. The temperature was increased to 120 ℃ at 10 ℃ · min ~ (-1) and kept at 120 ℃ for 1 min, then the temperature was increased to 280 ℃ at 2.5 ℃ · min ~ (-1). The results of DSC and HPLC were compared. Results: There was a good linear relationship between endothermic amount and sample weight (r = 0.999 0) in the range of 1.05 ~ 3.44 mg. The average recovery was 98.86% (RSD = 1.59%, n = 9). The results of HPLC and DSC were 97.77% and 97.80%, respectively. The relative average deviation of the two values was 0.015%. Conclusion: The DSC method has high accuracy and easy operation, and can be used together with HPLC method in the determination of hexamidine.