Departamento de Química Analítica, Instituto Universitario de Investigación en Química Fina y Nanoquímica IUIQFN, Universidad de Córdoba, Campus de Rabanales, Edificio Marie Curie (anexo), E-14071, Córdoba, Spain.
Departamento de Química Analítica, Instituto Universitario de Investigación en Química Fina y Nanoquímica IUIQFN, Universidad de Córdoba, Campus de Rabanales, Edificio Marie Curie (anexo), E-14071, Córdoba, Spain.
Anal Chim Acta. 2019 Jan 10;1046:132-139. doi: 10.1016/j.aca.2018.09.023. Epub 2018 Sep 15.
Supramolecular solvent (SUPRAS) extraction is gaining attraction as a sample treatment technique because of its great performance in terms of effectiveness, versatility, sample clean-up, quickness, cost and sustainability. However, the nature of SUPRASs, being formed by amphiphile molecules, results in poor compatibility with Gas Chromatography (GC). Here, we show the hitherto unexplored development of a SUPRAS with high thermal stability (HTS) suitable for subsequent direct analysis by Headspace (HS)-GC. This novel HTS-SUPRAS, based on poly-undecylenic acid -an oligomeric surfactant-, tetraglyme -a polar aprotic solvent with excellent chemical and thermal stability- and water, was fully characterized in terms of composition and physical properties such as thermal stability. Subsequently, the HTS-SUPRAS developed was further successfully applied, as a proof-of-principle, to the extraction and determination of residual solvents in pharmaceutical drugs, including several solvents (class 2C) whose analysis by HS-GC has been shown to be highly complex. Analytical performance was demonstrated as mandated by the International Council for Harmonisation of technical requirements for pharmaceuticals for human use (ICH). Furthermore, excellent recoveries (70-120%) and high precisions (<20%, expressed as relative standard deviations) were obtained for the analysis of several different drug formulations spiked with the analyzed 37 residual solvents at their respective maximum residue levels.
超分子溶剂（SUPRAS）萃取因其在有效性、多功能性、样品净化、快速性、成本和可持续性方面的出色表现而受到越来越多的关注，是一种样品处理技术。然而，由于 SUPRASs 是由两亲分子形成的，其与气相色谱（GC）的兼容性很差。在这里，我们展示了一种迄今为止尚未开发的具有高热稳定性（HTS）的 SUPRAS，适用于随后的顶空（HS）-GC 直接分析。这种基于聚十一烯酸（一种低聚物表面活性剂）、四甘醇（一种具有出色化学和热稳定性的非质子极性溶剂）和水的新型 HTS-SUPRAS，在组成和物理性质（如热稳定性）方面进行了全面表征。随后，作为原理验证，进一步成功地将开发的 HTS-SUPRAS 应用于药物中残留溶剂的提取和测定，包括几种溶剂（2C 类），其 HS-GC 分析已被证明非常复杂。分析性能符合人用药物技术要求国际协调理事会（ICH）的要求。此外，对于分析不同药物制剂中以各自最大残留水平添加的 37 种残留溶剂，回收率（70-120%）良好，精密度高（<20%，表示为相对标准偏差）。
