摘要
研究建立HPLC法测定VD3微胶囊干粉中VD3含量的方法。样品用甲醇超声提取,采用Hypersil BDS C18色谱柱(4.6 mm250 mm,5μm),甲醇为流动相,流速为1.0 mL/min,柱温为25℃,检测波长为264 nm,进样量20μL。在此提取和色谱条件下,空白溶液和空白辅料溶液对VD3的含量测定无干扰,系统适应性好;VD3浓度在8~12μg/mL范围内线性关系良好,相关系数r=0.9999;测定重复性、方法重复性和中间精密度RSD均小于1.0%;平均回收率在98%以上;耐用性RD均小于1.0%,含量测定稳定;24 h内稳定性好,RD均小于1.0%。该方法操作简单快捷、精密度高、回收率高,具有良好的系统适应性、重现性和应用性,可适用于VD3微胶囊干粉中VD3的含量检测。
A HPLC method for determination of VD3 in vitamin D3 microcapsule dry powder was established.Samples were extracted with methanol and ultrasound assisted.The sample was then separated by a Hypersil BDS C18(4.6 mm250 mm,5μm)column using methanol as the mobile phase,at 1.0 mL/min flow rate and 25℃column temperature.The content of D3 was determined by ultraviolet detector at the wavelength of 264 nm with the injection volume of 20μL.Under the above extraction and chromatographic conditions,the blank solution and the blank excipient solution had no interference on the determination of VD3,and showed a good system adaptability.VD3 has a good linear relationship in the range of 8~12μg/mL with the correlation coefficient of 0.9999.The RSD of sample repeatability,method repeatability and intermediate precision were less than 1.0%.The average recovery rate was more than 98%.The RD of durability were less than 1.0%,and the RD of stability were less than 1.0%within 24 h.The method has the advantages of simple and rapid operation,high precision,high recovery rate,good system adaptability,reproducibility and applicability.It can be used for the determination of VD3 in vitamin D3 microcapsule dry powder.
作者
王胜南
叶双明
刘爱琴
晁红娟
张莉华
WANG Sheng-nan;YE Shuang-ming;LIU Ai-qin;CHAO Hong-juan;ZHANG Li-hua(Zhejiang Medicine Co.,Ltd.Xinchang Pharmaceutical Factory,Xinchang 312500;Faculty of Food Science,Zhejiang Pharmaceutical College,Ningbo 315100)
出处
《中国食品添加剂》
CAS
2019年第9期159-163,共5页
China Food Additives
