ICOA, CNRS UMR 7311, University of Orleans, Pôle de chimie, rue de Chartres - BP 6759 45067, Orléans Cedex 2, France; Shimadzu France, Le luzard 2, Bat A, Bd Salvador Allende Noisiel, Marne-la-Vallée 77448, France.
ICOA, CNRS UMR 7311, University of Orleans, Pôle de chimie, rue de Chartres - BP 6759 45067, Orléans Cedex 2, France.
J Chromatogr A. 2024 Oct 25;1735:465323. doi: 10.1016/j.chroma.2024.465323. Epub 2024 Aug 30.
Plastic additives are introduced in plastic material formulations, along with organic polymers, to offer different properties such as stability, plasticity or color. However, plastic additives may migrate from the plastic material to the content (in case of plastic containers) or to the material in contact with the plastic, like human skin. In the case of plastic medical devices, this migration is of particular interest, as plastic additives may be deleterious to health. In the present paper, we examined the interest of combining supercritical fluid extraction (SFE) to supercritical fluid chromatography (SFC) hyphenated to mass spectrometry (MS) in an online system to characterize plastic additives in laboratory gloves, taken as samples of medical devices. A set of target compounds comprising 18 plasticizers, 4 antioxidants and 2 lubricants was defined and their detectability with MS was examined, where it appeared that electrospray ionization (ESI) provided better detectability than atmospheric pressure chemical ionization (APCI). After examining possible stationary phases with the help of Derringer desirability function, an isocratic chromatographic method (CO:methanol 95:5) was developed on Shim-pack UC Phenyl column. The extraction method was examined with a 3-level full factorial design of experiments to optimize the extraction temperature (40 °C) and pressure (200 bar). The online SFE-SFC-MS method was compared to offline methods where the samples were extracted with liquid solvents at atmospheric pressure or high pressure then analysed with SFC-MS. In all cases, offline methods showed significant contaminants (like the oleamide lubricant) issuing from laboratory plastic materials as nitrogen drying station, syringes and filters, while the online method allowed a complete elimination of laboratory contaminations. Furthermore, the online method saved time, solvents and laboratory consumables. It will also show that transferring a compressible fluid from a loading loop is favourable to high efficiency, as the resulting chromatographic peaks are much thinner than when transferring a liquid. Compared to injecting liquid heptane, the efficiency increase was 3.4-fold, while compared to injecting liquid methanol (a common practice in SFC), the efficiency increase was 13-fold. Finally, the additive composition of different laboratory gloves was compared.
塑料添加剂被引入塑料材料配方中，与有机聚合物一起使用，以提供不同的性质，如稳定性、可塑性或颜色。然而，塑料添加剂可能会从塑料材料迁移到内容物（如果是塑料容器）或与塑料接触的材料，如人体皮肤。在塑料医疗器械的情况下，这种迁移尤其值得关注，因为塑料添加剂可能对健康有害。在本文中，我们研究了将超临界流体萃取（SFE）与超临界流体色谱（SFC）结合，并与质谱（MS）在线系统相结合，以表征实验室手套中的塑料添加剂的方法，实验室手套被视为医疗器械的样本。定义了一组目标化合物，包括 18 种增塑剂、4 种抗氧化剂和 2 种润滑剂，并检查了它们与 MS 的检测能力，结果表明电喷雾电离（ESI）比大气压化学电离（APCI）提供了更好的检测能力。在用 Derringer 期望函数检查了可能的固定相之后，在 Shim-pack UC Phenyl 柱上开发了等度色谱方法（CO：甲醇 95：5）。通过 3 水平完全因子实验设计检查了提取方法，以优化提取温度（40°C）和压力（200 巴）。将在线 SFE-SFC-MS 方法与离线方法进行了比较，其中在大气压或高压下用液体溶剂提取样品，然后用 SFC-MS 进行分析。在所有情况下，离线方法都显示出显著的污染物（如油酸酰胺润滑剂），这些污染物来自实验室塑料材料，如氮气干燥站、注射器和过滤器，而在线方法则可以完全消除实验室污染。此外，在线方法节省了时间、溶剂和实验室消耗品。它还将表明，将可压缩流体从加载环转移到柱中有利于提高效率，因为所得色谱峰比转移液体时要薄得多。与注入液体庚烷相比，效率提高了 3.4 倍，而与注入液体甲醇（SFC 中的常见做法）相比，效率提高了 13 倍。最后，比较了不同实验室手套的添加剂组成。
