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目的:建立HPLC柱后衍生化法测定前列腺素E1(PGE1)脂肪乳中PGE1的含量。方法:采用固相萃取技术对样品进行预处理,使用Kromasil C18色谱柱(300 mm×4.6 mm,10μm),流动相为0.01 mol.L-1磷酸盐缓冲液(pH6.3)-乙腈(75∶25),流速1.0 mL.min-1,柱后反应液为1 mol.L-1氢氧化钾溶液,流速0.50 mL.min-1,反应温度为60℃,前列腺素B1(PGB1)为内标,检测波长为280 nm。结果:PGE1浓度在2.4～9μg.mL-1范围内线性关系良好,平均回收率(n=9)分别为97.2%(RSD=1.4%),98.4%(RSD=0.6%),97.8%(RSD=1.8%)。结论:此方法准确灵敏,可用于PGE1脂肪乳的质量控制。
OBJECTIVE: To establish a method for the determination of PGE1 in prostaglandin E1 (PGE1) fat emulsion by HPLC post column derivatization. Methods: The samples were pretreated by solid phase extraction (SPE) using Kromasil C18 column (300 mm × 4.6 mm, 10 μm) with a mobile phase of 0.01 mol·L-1 phosphate buffer (pH 6.3) : 25) at a flow rate of 1.0 mL · min-1. The post-column reaction was 1 mol·L-1 potassium hydroxide solution, the flow rate was 0.50 mL · min-1, the reaction temperature was 60 ℃ and the content of prostaglandin B1 Standard, detection wavelength of 280 nm. Results: The linear range of PGE1 was 2.4 ~ 9μg.mL-1. The average recoveries were 97.2% (RSD = 1.4%), 98.4% (RSD = 0.6%) and 97.8% = 1.8%). Conclusion: This method is accurate and sensitive and can be used for quality control of PGE1 fat emulsion.