| 引用本文: | 李勇,冯秀娥,梁泰刚,李青山.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[J].中国现代应用药学,2013,30(10):1104-1107. |
| LI Yong,FENG Xiu’e,LIANG Taigang,LI Qingshan.Determination of 2,5’-Dibromo-4,5,2’-trihydroxydiphenylmethanone and Its Related Substances by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2013,30(10):1104-1107. |
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| 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。 |
| 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 |
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| 基金项目:国家“863”计划项目(2013AA092903)；山西省自然科学基金(2013011060-2)；山西医科大学科技创新基金(01201116)；山西医科大学博士启动基金(B03201213) |
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| Determination of 2,5’-Dibromo-4,5,2’-trihydroxydiphenylmethanone and Its Related Substances by HPLC |
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LI Yong, FENG Xiu’e, LIANG Taigang, LI Qingshan
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School of Pharmaceutical Sciences, Shanxi Medical University, Taiyuan 030001, China
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| 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. |
| Key words: HPLC 2,5’-dibromo-4,5,2’-trihydroxydiphenylmethanone related substances content determination |
