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,5 μm);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 mL·min-1;柱温为 40℃;检测波长为210 nm;进样体积20 μL,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0.07 μg·mL-1、0.07 μg·mL-1、0.06 μg·mL-1、0.06 μg·mL-1,定量限分别为 0.15 μg·mL-1、0.15 μg·mL-1、0.15 μg·mL-1、0.15 μg·mL-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.
Abstract
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,5 μm)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 mL·min-1;the column temperature was 40℃;the detection wavelength was 210 nm;the injection volume was 20 μL.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 0.07 μg·mL-1,0.07 μg·mL-1,0.06 μg·mL-1,0.06 μg·mL-1,and the limits of quantification(LOQ)were 0.15 μg·mL-1,0.15 μg·mL-1,0.15 μg·mL-1,0.15 μg·mL-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.
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万方数据