佐米曲普坦的含量测定与有关物质检查的方法学研究

目的:建立佐米曲普坦的质量控制方法.方法:采用反相高效液相色谱法,以Shimadzu CLC-C8为分析柱,乙腈-10 mmol/L KH2PO4(25∶75,pH 7.5)溶液为流动相,检测波长229 nm测定佐米曲普坦的含量,并对其纯度进行考察.结果:建立的方法能够有效地分离合成原料、中间体、降解产物和其它有关杂质,含量测定结果与非水电位滴定法结果一致(P＞0.05).结论:高效液相色谱法可以有效地控制佐米曲普坦中微量有关杂质,非水滴定法和高效液相法均可有效地控制本品的含量.

HPLC determination of zolmitriptan and its related substances

OBJECTIVE: To develop an analytical method and quality control for determination of zolmitriptan and related substances. METHODS: Zolmitriptan and related substances were separated and determined on a shimadzu CLC-C(8) column (150 mm x 6 mm, 10 microm) with a mobile phase of acetonitrile-10 mmol/L phosphate buffer (25:75 pH 7.5) and a flow-rate of 1 ml/min; the UV-VIS detector was operated at 229 nm. RESULT: The limit of detection for the related substances was 0.5 ng on the zolmitriptan basis (S/N >3). Linear calibration curve was gene rated from 4 - 40 microg/ml with a correlation coefficient of 0.9999. The recovery rate of zolmitriptan was 99.1% with a standard deviation of 0.2%. The results of HPLC method were consistent with those of nonaqueous titration method. CONCLUSION: HPLC method is a rapid sensitive and accurate method for the determination of zolmitriptan and its related substances.