School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, China.
School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, China.
J Chromatogr A. 2019 Nov 22;1606:460382. doi: 10.1016/j.chroma.2019.460382. Epub 2019 Jul 18.
In this work, magnetic metal-organic frameworks-101 functionalized with graphite-like carbon nitride material (FeO/g-CN/MIL-101) has been simply prepared for the efficient enrichment of glucocorticoids in cosmetics. Due to the introduction of g-CN, the water stability of MIL-101 has been greatly improved. This composite material also showed better selectivity for glucocorticoids than those for polycyclic aromatic hydrocarbons and benzene compounds due to the hydrogen bonding effect with g-CN and the size-matching effect with MIL-101. When the prepared material was used as the sorbents in magnetic solid-phase extraction (MSPE) and coupled with ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS), a sensitive MSPE-UPLC-MS/MS method was developed. Under the optimal conditions, the calibration curves were linear over the concentration ranging from 0.01 to 2 μg/L with correlation coefficients (R) between 0.9915 and 0.9995. The limit of detection (LOD) was as low as 2 ng/L with the RSDs lower than 5.5%. The recoveries ranged from 77.3% to 113%. The LOD of glucocorticoids in real samples analysis was improved by nearly three orders of magnitude compared to current literature records. The results indicated that FeO/g-CN/MIL-101 could be used as MSPE extractant to determine glucocorticoids in complex cosmetics matrix.
在这项工作中，通过简单的方法制备了功能化石墨相氮化碳材料的磁性金属有机骨架-101（FeO/g-CN/MIL-101），用于高效富集化妆品中的糖皮质激素。由于引入了 g-CN，MIL-101 的水稳定性得到了极大的提高。由于与 g-CN 的氢键作用和与 MIL-101 的尺寸匹配效应，这种复合材料对糖皮质激素的选择性也优于多环芳烃和苯类化合物。当将制备的材料用作磁固相萃取（MSPE）中的吸附剂并与超高效液相色谱-质谱联用（UPLC-MS/MS）结合使用时，开发了一种灵敏的 MSPE-UPLC-MS/MS 方法。在最佳条件下，校准曲线在 0.01 至 2 μg/L 的浓度范围内呈线性，相关系数（R）在 0.9915 至 0.9995 之间。检测限（LOD）低至 2 ng/L，相对标准偏差（RSD）低于 5.5%。回收率在 77.3%至 113%之间。与当前文献记录相比，实际样品分析中糖皮质激素的 LOD 提高了近三个数量级。结果表明，FeO/g-CN/MIL-101 可用作 MSPE 萃取剂，用于复杂化妆品基质中糖皮质激素的测定。
