摘要
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.
作者
李立
杨龙华
王亮
Li Li Yang Longhua Wang Liang(Qingdao Institute for Food and Drug Control, Shandong Qingdao 266071, China)
出处
《中国药师》
CAS
2017年第9期1679-1681,共3页
China Pharmacist
