前列地尔脂微球注射液中游离药物浓度测定方法研究

摘要

Objective To develop a method for determining the free drug concentration in Lipid Microspheres Incorporating Prostaglandin E1. Methods The samples of Lipid Microspheres Incorporating Prostaglandin E1 were processed with different specifications of ultrafil-tration membrane and different centrifugation speeds,then the free drug concentration in the water phase was detected by the high per-formance liquid chromatography - mass spectrometry(HPLC - MS). Results The samples were processed by the 10 K ultrafiltration mem-brane and centrifugating for 30 min with 4 ℃ 5 000 r / min,then the free drug concentration was detected by HPLC - MS. The test samples were stable within 5 h,RSD = 0. 43% . The sample reproducibility was good. The mass concentration of prostaglandin E1(PGE1) in the range of 5 - 60 ng / mL showed the good linear relation. The linear equation was Y = 5. 758 6 X + 7. 127 5,r = 0. 997 2( n = 7). The lowest detection limit was 5 ng / mL. The average recovery rate was 96. 4% with RSD = 0. 88% . Conclusion This method can detect the free PGE1 concentration in Lipid Microspheres Incorporating Prostaglandin E1 rapidly,simply and effectively with good reproducibility.%目的：建立检测前列地尔脂微球中游离药物浓度的方法。方法采用不同规格的超滤膜、以不同离心速率对前列地尔脂微球注射液样品进行处理，高效液相色谱-质谱法检测水相中游离药物浓度。结果用10 K 超滤膜滤过、以5000 r / min 速率4℃离心30 min，对前列地尔脂微球注射液样品进行处理；采用高效液相色谱-质谱法检测水相中游离药物浓度，结果样品在5 h 内稳定，RSD 为0.43%，方法重现性良好。前列地尔质量浓度在5~60 ng / mL 范围内与峰面积线性关系良好，线性回归方程为 Y =5.7586 X +7.1275， r =0.9972( n =7)，最低检测限5 ng / mL。方法的平均回收率为96.4%，RSD 为0.88%。结论该法可快速简便有效地检测出前列地尔脂微球注射液中游离前列地尔的浓度，重现性良好。