高效液相色谱主成分对照品外标法测定硝酸甘油注射液有关物质  

Determination of Related Substances in Nitroglycerin Injection by HPLC Main Component Reference Substances External Standard Method

作　　者：颜慷祺 黄子健 李同根 卢瑞芯 黄泽丹 王涌杰 周小琴 Yan Kangqi;Huang Zijian;Li Tonggen;Lu Ruixin;Huang Zedan;Wang Yongjie;Zhou Xiaoqin(Guangzhou baiyunshan Mingxing pharmaceutical Co.,Ltd.,Guangzhou 510250,China)

机构地区：[1]广州白云山明兴制药有限公司,广东广州510250

出　　处：《广东化工》2024年第21期140-142,共3页Guangdong Chemical Industry

摘　　要：目的:建立高效液相色谱法测定硝酸甘油注射液中的有关物质。方法:采用色谱柱GL Sciences Inertsil ODS-3V C18(4.6 mm×250 mm,5μm);以0.1%磷酸水溶液为流动相A,甲醇为流动相B,梯度洗脱;流速为1.5 m L·min^(-1);柱温为40℃;检测波长为210 nm;进样体积20μL,以加校正因子的主成分对照品外标法计算杂质含量。结果:建立的色谱条件下,空白辅料无干扰,各杂质分离度良好,线性关系良好,杂质B、C、D和E检测限分别为0.07μg·m L^(-1)、0.07μg·m L^(-1)、0.06μg·m L^(-1)、0.06μg·m L^(-1),定量限分别为0.15μg·m L^(-1)、0.15μg·m L^(-1)、0.15μg·m L^(-1)、0.15μg·m L^(-1),平均回收率分别为103.6%、99.9%、106.7%、109.0%,RSD分别为0.6%、0.6%、1.5%、1.2%。结论:本方法操作简便、灵敏度高、专属性好,可用于硝酸甘油注射液有关物质的质量控制。Objective:To establish a HPLC method for the determination of related substances in nitroglycerin injection.Method:The separation was performed on a GL Sciences Inertsil ODS-3V C18 column (4.6 mm×250 mm,5μm) with 0.1%phosphoric acid as mobile phase A and methanol as mobile phase B in a gradient elution mode at a flow rate of 1.5 m L·min^(-1);the column temperature was 40℃;the detection wavelength was 210 nm;the injection volume was 20μL.The impurity content was calculated by external standard method of the principal component reference substance with the correction factor.Results:Under the established chromatographic parameters,there was no interference with the blank excipient,and the impurities were well separated with good linearity.The limits of detection(LOD) of impurities B,C,D and E were 0.07μg·m L^(-1),0.07μg·m L^(-1),0.06μg·m L^(-1),0.06μg·m L^(-1),and the limits of quantification (LOQ) were 0.15μg·m L^(-1),0.15μg·m L^(-1),0.15μg·m L^(-1),0.15μg·m L^(-1),with the average recoveries were 103.6%,99.9%,106.7%,109.0%,and the RSD were 0.6%,0.6%,1.5%,1.2%,respectively.Conclusion:The method is easy to operate,with high sensitivity and good specificity,and can be used for the quality control of related substances in nitroglycerin injection.

关 键 词：硝酸甘油注射液 有关物质 主成分对照品外标法 

分 类 号：TQ[化学工程]