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目的建立硝克柳胺含量和有关物质的高效液相色谱(high performance liquid chromatography,HPLC)测定方法。方法采用Inertsil C_8柱(250mm×4.6mm,5μm,GL Sciences Inc.);流动相为水-乙腈-四氢呋喃(50:50:1)(内含0.1%磷酸);流速为1.0mL/min;检测波长为330nm;柱温为30℃。结果在选定色谱条件下,主峰与有关物质峰分离度良好,硝克柳胺在0.02~1.0g/L浓度范围内线性关系良好(r=0.999 6);平均回收率为100.1%(n=9);检测限为0.1ng。结论该方法专属性强、灵敏度高、操作简便,可用于测定硝克柳胺的含量及有关物质。
Objective To establish a high performance liquid chromatography (HPLC) method for the determination of the content of nodularlamine and its related substances. Methods Inertsil C_8 column (250 mm × 4.6 mm, 5 μm, GL Sciences Inc.) was used. The mobile phase was water-acetonitrile-tetrahydrofuran (50:50: 1) The wavelength is 330nm; the column temperature is 30 ℃. Results Under the selected chromatographic conditions, the separation peak of the main peak from the related substances was good. The calibration curve of nodularline was linear in the concentration range of 0.02-1.0 g / L (r = 0.999 6). The average recovery was 100.1% (n = 9); detection limit of 0.1ng. Conclusion The method is specific, sensitive and easy to operate. It can be used for the determination of the content of nodularlamine and its related substances.