烟酰胺片含量及有关物质测定方法改进  

Improvement of Determination Method of Nicotinamide Content and Related Substances in Nicotinamide Tablets

作　　者：李志远 刘屹 左文松 LI Zhiyuan;LIU Yi;ZUO Wensong(Yunnan Institute for Food and Drug Control,Kunming,Yunnan,China 650106)

机构地区：[1]云南省食品药品监督检验研究院,云南昆明650106

出　　处：《中国药业》2019年第9期35-38,共4页China Pharmaceuticals

摘　　要：目的建立测定烟酰胺片含量及有关物质的高效液相色谱(HPLC)法。方法色谱柱采用UITimate XB-C18柱(250 mm×4. 6 mm,5μm),流动相为甲醇-p H 6. 0的0. 05 mol/L醋酸铵溶液(10∶90),柱温为30℃,流速为1. 0 m L/min,进样量为20μL,检测器为PDA。结果按新建HPLC法测定73批样品的含量,与2015年版《中国药典(二部)》紫外分光光度(UV)法测定结果无显著差异(t=0. 79,P>0. 05)。按2015年版《中国药典(二部)》薄层色谱(TLC)法检测,均未检出烟酸及其他杂质;按新建HPLC法测定,均检出烟酸杂质,大部分样品检出其他杂质。结论所建立的方法简便、准确、可靠,可用于烟酰胺片含量及有关物质测定,同时能高效、快捷地区分样品间杂质谱的差异,并能对各杂质进行定量。Objective To establish an HPLC method for the content determination of nicotinamide and related substances in Nicotinamide Tablets.Methods The chromatographic column was UITimate XB-C18 column(250 mm×4.6 mm,5μm),the mobile phase was methanol-0.05 mol/L ammonium acetate with pH of 6.0(10∶90),the column temperature was 30℃,the flow rate was 1.0 mL/min,the sample size was 20μL,the detector was PDA.Results According to the newly established HPLC method,the content of 73 batches of samples was determined,and the results were not significantly different from that determined by the UV method in the Chinese Pharmacopoeia(VolumeⅡ,2015 edition)(t=0.79,P>0.05).The 73 batches of samples were tested according to the TLC method in Chinese Pharmacopoeia(VolumeⅡ,2015 edition),no niacin and other impurities were detected.According to the newly established HPLC method,nicotinic acid impurities were detected,and the other impurities were detected in most of the samples.Conclusion The established HPLC method is simple,accurate and reliable.It can be used for the content determination of nicotinamide and related substances in Nicotinamide Tablets.It can also efficiently and quickly distinguish the difference of impurity mass spectra among the samples,and quantify each impurity.

关 键 词：烟酰胺片 高效液相色谱法 烟酰胺 有关物质 含量测定 中国药典 

分 类 号：R927.2[医药卫生—药学] R977.2