梯度洗脱HPLC法双波长测定呋喃唑酮中的相关物质

Determination of related substances in furazolidone by gradient elution HPLC with double UV wavelengths

目的:建立测定呋喃唑酮中5-硝基糠醛二乙酸酯及其他相关物质的方法。方法:采用反相高效液相色谱法,色谱柱为Alltima C18(150 mm×4.6 mm,5μm),流动相为水-乙腈,梯度洗脱[0 min(90%水)→10 min(50%水)→20 min(95%水)→30min(95%水)→35 min(90%水)],流速1.0 mL.min-1,检测波长为303 nm(5-硝基糠醛二乙酸酯)和210 nm(其他相关物质)。结果:呋喃唑酮与5-硝基糠醛二乙酸酯及其强制破坏产生的降解产物均分离良好;5-硝基糠醛二乙酸酯线性范围为0.2516～3.744μg.mL-1,平均回收率(n=9)为100.7%;呋喃唑酮和5-硝基糠醛二乙酸酯最低检测量分别为1.53 ng和0.20 ng;供试品溶液至少8 h内稳定。结论:本法专属性强,操作方便,测定准确,灵敏度高,可作为呋喃唑酮的质量控制方法。

Objective：To establish a method for determination of 5-nitro-2-furaldehyde diacetate and other related substances in furazolidone.Methods：An Alltima C18 column（150 mm×4.6 mm,5 μm） was adopted.The mobile phase was water-acetonitrile with gradient elution[0 min（90% water）→10 min（50% water）→20 min（95% water）→30 min（95% water）→35 min（90% water）];5-nitro-2-furaldehyde diacetate and other related substances were determined with double UV wavelengths,which were 303 nm for 5-nitro-2-furaldehyde diacetate and 210 nm for other related substances.Results：The resolution between furazolidone peak and other peaks was good.The linear range of 5-nitro-2-furaldehyde diacetate was 0.2516-3.744 μg·mL-1 and the average recovery（n=9） was 100.7%;The detection limits of furazolidone and 5-nitro-2-furaldehyde diacetate were 1.53 ng and 0.20 ng,respectively.The test solution was stable within 8 h.Conclusion：The method is specific,convenient,accurate,sensitive,and can be used for the quality control of furazolidone.