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目的:建立测定大鼠血浆中甲磺酸二氢麦角毒碱的反相高效液相荧光检测方法。方法:血浆样品预处理采用乙腈直接沉淀法去除蛋白质。采用 L-7000型高效液相色谱仪,Phenomenex C_(18)柱(250 mm×4.6 mm,5μm);流动相为水-乙腈-三乙胺(32:18:1),流速为1.1 mL·min~(-1);荧光检测波长:λ_(Ex)=290 nm,λ_(Ex)=348 nm;柱温:30℃;进样量:50μL。外标法峰面积定量。结果:血浆中甲磺酸二氢麦角毒碱能得到较好的分离,无明显的干扰峰。测定方法在1.0～200.0 ng·mL~(-1)范围内具有良好的线性关系,方法回收率为96.2%～100%,日内、日间 RSD 均小于15%,最低检测浓度为1.0 ng·mL~(-1),最低检测限为50 pg。结论:本法灵敏、准确、快速,适用于甲磺酸二氢麦角毒碱鼻腔喷雾剂的药物动力学和生物利用度的研究。
Objective: To establish a method for the determination of dihydrocoxydine methanesulfonate in rat plasma by reversed-phase high performance liquid chromatography. Methods: Plasma samples were pre-treated with acetonitrile to remove protein directly. Phenomenex C_ (18) column (250 mm × 4.6 mm, 5 μm) was used on a L-7000 high performance liquid chromatograph. The mobile phase was water-acetonitrile-triethylamine The fluorescence detection wavelength was λ_ (Ex) = 290 nm and λ_ (Ex) = 348 nm. The column temperature was 30 ℃. The injection volume was 50 μL. External standard peak area of quantitative. Results: Plasma ergocaline mesylate can be better separated without obvious interference peak. The method has good linearity in the range of 1.0 ~ 200.0 ng · mL ~ (-1), the recovery rate is 96.2% ~ 100%, the RSD is less than 15%, the minimum detectable concentration is 1.0 ng · mL ~ (-1), the lowest detection limit is 50 pg. Conclusion: This method is sensitive, accurate and rapid, suitable for pharmacokinetics and bioavailability of dihydrocelyl mesylate nasal spray.