3,3'-二氨基-4,4'-氧化偶氮呋咱的纯度测定及杂质表征

Determination of 3,3'-Diamino-4,4'-azoxyfurazan and Characterization of Impurities

建立了3,3'-二氨基-4,4'-氧化偶氮呋咱(DAOAF)的高效液相色谱分析方法,采用质谱对其中含有的杂质进行了表征。结果表明,优化后的色谱条件为:Zorbax SB-C18(250 mm×4.6 mm,5.0μm)柱;流动相乙腈/水(体积比为40/60);流速0.8 m L·min^(-1);柱温25℃;UV检测波长为230 nm。进样体积10μL。在优化色谱条件下,DAOAF和其中的杂质得到有效分离。DAOAF在10.02~100.20 mg·L^(-1)质量浓度范围内,DAOAF校准曲线的线性关系良好,线性相关系数为0.9990。DAOAF中的主要杂质为二氨基乙二肟、3,4-二氨基呋咱和3,3'-二氨基-4,4'-偶氮呋咱。该方法灵敏度高,重现性好,可用于DAOAF产品中有关物质的检测分析。

A high performance liquid chromatography to analyze 3,3′-diamino-4,4′-azoxyfurazan（DAOAF） was established and characterization of impurities trapped in the DAOAF product was carried out by MS. Results show that the chromatographic conditions after optimization are： chromatographic column, ZorbaxSB-C18（250 mm×4.6 mm, 5.0 μm） column; mobile phase, acetonitrile/water （V∶V=40∶60）; flow rate, 0.8 mL·min-1; column temperature, 25 ℃; wavelength, 230nm; injection volume,10 μL. Under the optimized chromatographic conditions, DAOAF and impurities in DAOAF are effectively separated. The calibration curves of DAOAF within the mass concentration of 10.02-100.20 mg·L-1 have good linearity with the linear correlation coefficient of 0.9990. The main impurities in DAOAF are diaminoglyoxime, 3,4-diaminofurazan and 3,3′-diamino-4,4′-azofurazan. The method has high sensitivity and good reproducibility, can be used for the determination of the related substances in the product of DAOAF.