HPLC测定2,5’-二溴-4,5,2’-三羟基二苯甲酮原料药的含量及有关物质

Determination of 2,5’-Dibromo-4,5,2’-trihydroxydiphenylmethanone and Its Related Substances by HPLC

关键词:  高效液相色谱法  2，5’-二溴-4，5，2’-三羟基二苯甲酮  有关物质  含量测定

Key words:  HPLC  2,5’-dibromo-4,5,2’-trihydroxydiphenylmethanone  related substances  content determination

摘要:

目的 建立HPLC测定海洋来源活性化合物2,5’-二溴-4,5,2’-三羟基二苯甲酮原料药(LM49)的含量及有关物质的方法。方法 采用Diamonsil C₁₈(250 mm×4.6 mm，5 μm)色谱柱，甲醇-乙腈-水(磷酸调pH至3.0)(70∶10∶20)为流动相，检测波长为261 nm，流速0.8 mL·min^-1，柱温25 ℃。结果 主峰能与杂质峰达到良好分离，LM49在浓度1.0~100 mg·L^-1内线性关系良好(r=0.999 9)，最低检测限为0.02 mg·L^-1，平均回收率为99.8%(RSD=0.88%)。结论 本法简便、快速、准确，可用于LM49原料药的含量及有关物质的测定。

Abstract:

OBJECTIVE To establish an HPLC method for the determination of 2,5’-dibromo-4,5,2’-trihydroxydiphenyl- methanone(LM49) and its related substances. METHODS HPLC method was carried on a column of Diamonsil C₁₈ column (250 mm × 4.6 mm, 5 μm) with the mobile phase of methanol-acetonitrile-water (adjusted to pH 3.0 with phosphoric acid) (70∶10∶20) at the flow rate of 0.8 mL·min^-1 and the detection wavelength was set at 261 nm. The column temperature was 25 ℃. RESULTS LM49 was completely separated from the impurities. A good linearity(r=0.999 9) of LM49 was obtained at the concentration range of 1.0-100 mg·L^-1. The minimal detection limit was 0.02 mg·L^-1. The average recovery of method was 99.8%(RSD=0.88%). CONCLUSION The analytical method is simple, rapid, sensitive and accurate for the determination of LM49 and its related substances.