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目的:建立一种高效、快速、样品在线预处理的柱切换柱后衍生高效液相色谱法,用以测定脂质体微球类药物前列地尔注射液中主药的含量。方法:采用Merck LiChroCART25-4色谱柱(25 mm×4 mm,5μm)为预处理柱,以无水乙醇为洗脱液,流速为2.0 mL·min-1,柱温60℃;以LiChrospher100 RP-18e C18色谱柱(25 mm×4 mm,5μm)为压力替换柱,用以平衡系统压力,柱温60℃;采用Agilent Zorbax SB C18色谱柱(250 mm×4.6 mm,5μm)为分析柱,以0.0067 mol·L-1磷酸盐缓冲液(取磷酸二氢钾9.07 g,加水1000 mL使溶解,用0.1 mol·L-1氢氧化钠溶液调节pH至6.3)-乙腈(5∶2)为流动相,流速1.0 mL·min-1,检测波长278 nm,柱温60℃;以1 mol·L-1氢氧化钾溶液为柱后反应液,流速0.5 mL·min-1;进样量20μL。结果:前列地尔浓度在0.25~12.0μg·mL-1范围内线性关系良好(r=0.9993);平均回收率(n=9)为99.25%。结论:本方法经方法学验证操作简便、准确,可作为前列地尔注射液含量测定的分析方法。
OBJECTIVE: To establish a high-performance, rapid, on-line pretreatment column-switched post-column derivatization high performance liquid chromatography for the determination of the main drug content in the liposome microsphere drug prostaglandin injection. METHODS: Merck LiChroCART25-4 column (25 mm × 4 mm, 5 μm) was used as a pretreatment column with absolute ethanol as eluent at a flow rate of 2.0 mL · min-1 and a column temperature of 60 ° C. LiChrospher 100 RP-18e C18 column (25 mm × 4 mm, 5 μm) is a pressure-exchange column to balance the system pressure with a column temperature of 60 ° C. An Agilent Zorbax SB C18 column (250 mm × 4.6 mm, 5 μm) The analytical column was eluted with 0.0067 mol·L-1 phosphate buffer (potassium dihydrogen phosphate 9.07 g, dissolved in 1000 mL of water and adjusted to pH 6.3 with 0.1 mol·L-1 sodium hydroxide solution) -acetonitrile (5: 2) as the mobile phase at a flow rate of 1.0 mL · min-1 with a detection wavelength of 278 nm and a column temperature of 60 ℃. The column was treated with 1 mol·L-1 potassium hydroxide solution at a flow rate of 0.5 mL · min-1 Sample volume 20μL. Results: The linear range of alprostadil was 0.25 ~ 12.0μg · mL-1 (r = 0.9993). The average recovery was 99.25% (n = 9). Conclusion: The method is validated by methodological method and is simple and accurate. It can be used as an analytical method for the determination of alprostadil injection.