差示扫描量热法测定甘露六烟酯原料药含量

Determination of Mannityl Nicotinate API by DSC

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 DSC method for the determination of mannityl nicotinate. Methods ： Indium was used to correct the instrument including temperature correction and heat flow correction. The atmosphere was nitrogen and the flow rate was 20 ml·min^-1. The sample volume was 1-3.5 mg with precision reached to 0.0ling. The initial temperature was 30 ℃, raised to 120 ℃ at the rate of 10 ℃·min^-1, maintaining for 1 rain at 120 ℃, and raised to 280 ℃ at the rate of 2.5 ℃·min^-1. The results of DSC and HPLC were compared. Results： Mannityl nicotinate had a good linear relationship between the heat absorption and the amount of sample within the range of 1.05-3.44 mg （r =0.999 0）. The average recovery was 98.86% （RSD=.59% ,n=9）. The content of niacin detected by HPLC and DSC was 97.77% and 97.80%, respectively, and the relative mean deviation of the two values was 0. 015%. Conclusion： The DSC method is accurate and rapid, and can be used for the determination of mannityl nicotinate like HPLC.