反相高效液相色谱法测定硝酸甘油气雾剂有关物质和硝酸甘油含量

RP-HPLC determination of nitroglycerin aerosol and its related substances

目的:建立高效液相色谱法测定硝酸甘油气雾剂有关物质和硝酸甘油含量。方法:采用Kromasil C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-水(50∶50)为流动相,流速1 mL·min-1,在215 nm波长处检测,分别用自身对照法和外标法计算硝酸甘油气雾剂有关物质和硝酸甘油含量。结果:4批样品的最大单个杂质分别为0.5%,0.5%,0.3%,0.7%;杂质总量分别为1.0%,1.3%,0.8%,2.2%;有关物质线性范围为0.27～26.59μg·mL-1(r=0.9999);硝酸甘油含量线性范围为20.23～202.27μg·mL-1(r=0.9997),平均回收率(n=9)为102.6%,最低检出限为0.61 ng。结论:实验证明该法准确可行,为硝酸甘油气雾剂质量标准修订提供了参考。

Objective：To establish an HPLC method for the determination of the related substances and nitroglycerin content of nitroglycerin aerosol.Methods： The chromatographic column was Kromasil C18（250 mm×4.6 mm,5 μm） column,with acetonitrile-water（50∶50） as mobile phase;the flow rate was 1 mL·min-1 and the detection wavelength was 215 nm.The related substances were quantified by self-calibrated method and the content was quantified by external standard.Results： Four batches of samples were tested and the content of the maximum individual impurity was 0.5%,0.5%,0.3% and 0.7%,respectively and the total content was 1.0%,1.3%,0.8% and 2.2%,respectively;The linear range of related substances was 0.27-26.59 μg·mL-1（r=0.9999）;The linear range of nitroglycerin was 20.23-202.27 μg·mL-1（r=0.9997）,the average recovery（n=9） was 102.6%,and the detection limit was 0.61 ng.Conclution： This method is accurate and feasible.It provided a reference for revising the quality standards of nitroglycerin aerosol.