Department of Pharmaceutical Analysis, School of Pharmacy, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430030, China; Department of Pharmacy, Union Hospital, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430022, China.
Department of Pharmaceutical Analysis, School of Pharmacy, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430030, China.
J Chromatogr A. 2020 Jul 5;1622:461137. doi: 10.1016/j.chroma.2020.461137. Epub 2020 Apr 20.
In this study, conventional Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method was modified by magnetic solid-phase extraction (MSPE) for purification/pre-concentration of eleven estrogens and estrogen mimics from the extracts of pork and chicken muscles, prior to dansyl chloride (DNS-Cl) derivatization coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) assay. Dual octadecyl- and 2-aminoethyl-3-aminopropyl- groups functionalized mesoporous silica core-shell magnetic nanoparticles (C/NH-FeO@mSiO MNPs) were synthesized and employed as MSPE sorbent with remarkable aqueous compatibility in comparison with conventional C functionalized sorbent. The proposed MSPE is easier to handle than the traditional SPE purification process in QuEChERS method. The lab-prepared MNPs were characterized by transmission electron microscope (TEM), brunner-emmet-teller (BET), dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Pre-column derivatization was conducted to significantly enhance the sensitivity of the analytes in MS/MS via analyzing their derivatives in positive ion mode instead of analyzing their original forms in negative ion mode. Under the optimal sample pretreatment and instrumental analysis conditions, the approach showed low limits of detection (LODs, 0.02‒3.00 µg kg), appropriate recoveries (81.1‒115.4%) and acceptable precisions (0.48‒15.1%, n = 6), with good feasibility and future prospect of trace compounds analysis in complex food samples.
在这项研究中，对传统的快速、简便、廉价、有效、坚固和安全（QuEChERS）方法进行了改进，通过磁固相萃取（MSPE）对猪肉和鸡肉肌肉提取物中的 11 种雌激素和类雌激素进行净化/预浓缩，然后进行丹磺酰氯（DNS-Cl）衍生化，与超高效液相色谱-串联质谱（UHPLC-MS/MS）联用。合成了双十八烷基和 2-氨基乙基-3-氨基丙基功能化介孔硅核壳磁性纳米粒子（C/NH-FeO@mSiO MNPs），并将其用作 MSPE 吸附剂，与传统的 C 功能化吸附剂相比，具有显著的亲水性。与 QuEChERS 方法中的传统 SPE 净化过程相比，所提出的 MSPE 更易于处理。实验室制备的 MNPs 通过透射电子显微镜（TEM）、布鲁纳-埃梅特-泰勒（BET）、动态光散射（DLS）、傅里叶变换红外光谱（FT-IR）、热重分析（TGA）和振动样品磁强计（VSM）进行了表征。通过在正离子模式下分析衍生化合物而不是在负离子模式下分析其原始形式，预柱衍生化可显著提高分析物在 MS/MS 中的灵敏度。在最佳的样品预处理和仪器分析条件下，该方法具有较低的检出限（LOD，0.02-3.00μg kg）、适当的回收率（81.1-115.4%）和可接受的精密度（0.48-15.1%，n=6），具有良好的可行性和在复杂食品样品中痕量化合物分析的未来前景。
