Development and validation of a novel UPLC-ELSD method for the assessment of lipid composition of nanomedicine formulation
Development and validation of a novel UPLC-ELSD method for the assessment of lipid composition of nanomedicine formulation
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DOI：
10.1016/j.ijpharm.2019.05.038
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发表时间：
2019-07-20
影响因子：
5.8
通讯作者：
Couffin, Anne-Claude
中科院分区：
文献类型：
--
作者：
Varache, Mathieu;Ciancone, Mathieu;Couffin, Anne-Claude
结合甘油酯、聚乙二醇（PEG）-硬脂酸酯和磷脂的脂质纳米载体在体内诊断、体内成像、活化或非活化靶向药物递送方面引起了极大的关注。为了质量控制的目的，需要开发适当的方法来定量其脂质成分。在本研究中，我们开发了一种用于配制的纳米颗粒中的脂质定量的分析方法。使用两步梯度洗脱程序通过RP-UPLC-ELSD在单次运行中分析PEG-硬脂酸酯和甘油酯，而使用SPE硅胶柱分离后通过HILIC-UPLC-ELSD完成磷脂分析。使用分离的化合物和市售脂质标准品，使用二阶多项式生成校准曲线，以获得每种脂质辅料的定量评价。所有分析物的日内精密度的相对标准偏差在0.9%至5.3%之间，回收率在83.5%至112.2%之间。成功实施了所述方法，以研究配制脂质辅料在长期储存和加速条件下的生产工艺和稳定性。测定制剂脂质产率，发现等于82.5%。
Lipid nanocarriers incorporating glycerides, polyethylene glycol (PEG)-stearates and phospholipids have attracted great attention for in vivo diagnostic, in vivo imaging, activated or non-activated targeted drug delivery. For quality control purposes, the development of appropriate methods for the quantification of their lipid components is needed. In the present study, we developed an analytical method for lipid quantification in formulated nanoparticles. PEG-stearates and glycerides were analyzed in a single run by RP-UPLC-ELSD using a two-step gradient elution program, while the analysis of phospholipids was accomplished by HILIC-UPLC-ELSD after isolation using an SPE silica column. Using both isolated compounds and commercial lipid standards, calibration curves were produced using second-order polynomials to attain the quantitative evaluation of each lipid excipient. Relative standard deviation of all analytes was between 0.9% and 5.3% for intra-day precision and recovery ranged from 83.5% to 112.2%. The presented method was successfully implemented to study the manufacturing process and stability of the formulated lipid excipients during long-term storage and accelerated conditions. The formulation lipid yield was determined and found equal to 82.5%.