超高效液相色谱法测定Menaquinone-7原料药主成分及有关物质  

Determination of Principal Compound and Related Substances in Raw Material Drug of Menaquinone-7 by UPLC

作　　者：宋怡 孔凡建 李银科[2] 王泉[2] 

机构地区：[1]云南省玉溪市食品药品检验所,玉溪653100 [2]玉溪师范学院,玉溪653100

出　　处：《理化检验（化学分册）》2017年第12期1381-1385,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金(21562044)

摘　　要：Menaquinone-7原料药在避光条件下经无水乙醇超声溶解后,采用Agilent Eclipse plus C_(18)色谱柱(2.1mm×50mm,1.8μm)分离主成分及有关物质,以甲醇-水(98+2)混合液为流动相,分别在波长246,270nm处测定主成分及有关物质。Menaquinone-7的线性范围在0.005~0.400g·L^(-1)内,检出限(3S/N)为0.1mg·L^(-1)。加标回收率在98.8%~100%之间,测定值的相对标准偏差(n=6)小于1.0%。测得两批Menaquinone-7原料药中主成分的质量分数分别为98.0%,98.2%,单个杂质质量分数小于0.5%,杂质总质量分数小于1.0%。Raw material drug of Menaquinone-7 was dissolved ultrasonically with ethanol in the dark,and then the principal compound and related substances in the sample were separated on an Agilent Eclipse plus C_（18） chromatographic column（2.1 mm×50 mm,1.8μm）.The mobile phase was methanol-water（98＋2）solution,and the detection wavelengths were 246,270 nm for the determination of principal compound and related substances,respectively.The linearity range of Menaquinone-7 was 0.005-0.400 g·L^（-1）,with detection limit（3 S/N）of0.1 mg·L^（-1）.Recovery rates obtained by standard addition method were in the range of 98.8%-100% and RSDs（n=6）were less than 1.0%.The contents of the principal compound in 2 batches of Menaquinone-7 raw material drug were 98.0% and 98.2%.The mass fraction of single impurity was less than 0.5%,and the mass fraction of total impurities was less than 1.0%.

关 键 词：超高效液相色谱法 Menaquinone-7 主成分 有关物质 

分 类 号：O657.7[理学—分析化学]