HPLC-CAD测定羟基脲胶囊含量及有关物质

Determination of the Content and the Related Substances of Hydroxycarbamide Capsules by HPLC-CAD

关键词:  羟基脲胶囊  有关物质  含量  脲

Key words:  hydroxycarbamide capsule  related substance  content  carbamide

摘要:

目的 建立测定羟基脲胶囊含量及有关物质检查的HPLC-CAD方法。方法 采用Phenomenx Luna^® NH₂柱（250 mm×4.6 mm，10 μm，100Ǻ），柱温为40℃；以乙腈-水（82：18）为流动相，流速为1.0 mL·min^-1，检测器为电雾式检测器，雾化温度50℃，进样量10 μL。结果 在选定的色谱条件下，主峰与各杂质峰均能良好分离。采用外标法计算羟基脲胶囊的含量，采用主成分自身对照法计算脲的含量；羟基脲和脲分别在0.304 8~1.270 0 mg·mL^-1（r=0.999 8）、0.241 1~1.004 6 mg·mL^-1（r=1.000 0）内与峰面积呈良好线性关系。脲的检测限和定量限分别为2.82 ng和8.46 ng。结论 本方法操作简便，专属性强，结果可靠，可用于羟基脲胶囊的含量及有关物质的测定。

Abstract:

OBJECTIVE To establish an HPLC-CAD method for determination of the content and the related substances of hydroxycarbamide capsules. METHODS The determination was carried out on a Phenomenex Luna^® NH₂(250 mm×4.6 mm, 10 μm, 100Ǻ) column at 40℃, with acetonitrile-water(82:18) as mobile phase at a flow rate of 1.0 mL·min^-1. The detector of charged aerosol detection was applied with a high nebulization temperature at 50℃, the injection volume was 10 μL. RESULTS Under the selected chromatographic conditions, related substances were completely separated from the principal component. The content of hydroxycarbamide capsules was calculated by the external standard method of the reference substance, and the content of carbamide was calculated by the self-control method of the main component. Hydroxycarbamide and carbamide showed a good linear relationship with the peak area in the concentration range of 0.304 8-1.270 0 mg·mL^-1(r=0.999 8) and 0.241 1-1.004 6 mg·mL^-1(r=1.000 0), respectively. The detection limits and quantitation limits of carbamide were 2.82 ng and 8.46 ng, respectively. CONCLUSION The method is simple, specific and reliable, and can be used for the determination of the content of hydroxycarbamide capsules and related substances.