HPLC-ELSD测定多西他赛注射用浓溶液中溶血磷脂酰乙醇胺、溶血磷脂酰胆碱的含量

Determination of Lyso-phosphatidylethanolamine and Lyso-phosphatidylcholine in Docetaxel Concentrated Solution for Injection

关键词:  多西他赛注射用浓溶液  溶血磷脂酰乙醇胺  溶血磷脂酰胆碱  高效液相色谱-蒸发光散射法  含量测定

Key words:  Docetaxel Concentrated Solution for Injection  lyso-phosphatidylethanolamine  lyso-phosphatidylcholine  HPLC-ELSD  content determination

摘要:

目的 建立同时测定多西他赛注射用浓溶液中的溶血磷脂酰乙醇胺(LPE)、溶血磷脂酰胆碱(LPC)含量的HPLC-ELSD。方法 采用YMC Pack PVA-Sil(150 mm×2 mm，5 μm)色谱柱，以三氯甲烷为流动相A、甲醇-水(93.5∶6.5)为流动相B，梯度洗脱，流速为0.4 mL·min^-1，柱温为25 ℃，蒸发光散射检测器检测，检测器漂移管温度：100 ℃，雾化气：空气，气体流量为2.0 L·min^-1。结果 LPE和LPC峰面积的对数与相应的浓度的对数呈良好的线性关系，线性范围分别为0.203~0.811 μg(r=0. 999 0)和0.407~6.102 μg(r=0.999 6)，LPE 3个浓度的平均加样回收率分别为104.1%，95.1%，101.6%，RSD分别为3.8%，0.3%，2.4%，LPC 3个浓度的平均回收率分别为108.7%，104.5%，105.5%，RSD分别为1.0%，3.0%，2.6%。结论 该法简单、准确、重复性好，可用于多西他赛注射用浓溶液中大豆磷脂分解产物的质量控制。

Abstract:

OBJECTIVE To develop an HPLC-ELSD method for the determination of lyso-phosphatidylcholine(LPC) and lyso-phosphatidylethanolamine(LPE) in Docetaxel Concentrated Solution for Injection. METHODS It was separated with YMC Pack PVA-Sil(150 mm×2 mm, 5 μm) by gradient elution with chloroform as mobile phase A and methanol-water (93.5∶6.5) as mobile phase B at a flow rate of 0.4 mL·min^-1. The column temperature was kept at 25 ℃ for separation. The detector was ELSD, of which the drift tube temperature was maintained at 100 ℃ and the flow rate of carrier gas air was kept at 2.0 L·min^-1. RESULTS The linear response was calculated by logarithm. The calibration curves were linear in the range of 0.203-0.811 μg(r=0.999 0) for LPE and 0.407-6.102 μg(r=0.999 6) for LPC. The average recovery for LPE was 104.1%, 95.1%, 101.6%, RSD=4.6%; and the average recovery for LPC was 108.7%, 104.5%, 105.5%, RSD=2.7%. CONCLUSION The established method is simple, accurate and reproducible, which can be used for the quality control of Docetaxel Concentrated Solution for Injection.