HPLC-ELSD法测定前列地尔纳米乳注射液中溶血磷脂的含量

HPLC-ELSD determination of lysophosphatidylcholine in Alprostadil nano emulsion injection

目的采用HPLC-ELSD法测定前列地尔纳米乳注射液中溶血磷脂含量。方法建立HPLC-ELSD测定溶血磷脂的方法,色谱柱为:Intertsil?SIL-100A(4.6 mm×250 mm,5μm),以甲醇-冰醋酸(500∶10,三乙胺调节pH至6.0)为流动相。联合ELSD,控制漂移管温度:85℃,用氮气作为载气,流量:1.6 L/min。结果在选定的条件下,溶血磷脂与样品中其他组分分离良好。溶血磷脂检测限(LOD)为36 ng;溶血磷脂在3.6~180μg/m L范围内,峰面积的对数与浓度的对数呈良好的线性关系(R2=0.999 4);日内和日间精密度RSD均<2%(n=6);平均回收率为100.88%,RSD为2.51%(n=9),3批样品溶血磷脂含量分别为:0.311 mg/m L,0.326 mg/m L,0.325 mg/m L。结论本法简便易行,重复性好,灵敏度高,专属性强,可用于前列地尔纳米乳注射液中溶血磷脂的含量测定。

Objective To develop an HPLC-ELSD method for determination of lysophosphatidyl choline in Alprostadil nanoemulsion injection.Methods The HPLC-ELSD method was performed on an Intertsil?SIL-100A column(4.6mm×250mm,5μm)with methanol-aceticacid(500∶10,adjusted pH6.0with triethylamine)as mobile phase.The detector was ELSD,of which the drift tube temperature was maintained at85℃and the flow rateof carrier gas was kept at1.6mL/min.Results Under the described condition,lysophosphatidylcholine was completely separated from other componentsin alprostadil nano emulsion injection.The LOD of lysophosphatidyl choline was36ng.In the range of3.6～180μg/mL,the peak area of logarithmicof lysophosphatidylcholine had good linear relationship with the logarithm of concentration(R2=0.9994).Both intra-and inter-day precision RSDwere<2%(n=6)and the average recovery was100.88%,RSD=2.51%(n=9).Lysophosphatidylcholine contents in3batches of samples,respectively:0.311mg/mL,0.325mg/mL,0.326mg/mL.Conclusion This methods have good repeatability,high sensitivity,strong specificity and can beused for determination of lysophosphatidyl choline in Alprostadil nanoemulsion injection.