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基于超声辅助离子液体捕集-微固相萃取的胺功能化双模态介孔硅纳米粒子在人生物样本中的铅分析。

A lead analysis based on amine functionalized bimodal mesoporous silica nanoparticles in human biological samples by ultrasound assisted-ionic liquid trap-micro solid phase extraction.

机构信息

Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran, Iran.

Department of Medical Nanotechnology, Faculty of Advanced Sciences & Technology, Pharmaceutical Sciences Branch, Islamic Azad University (IAUPS), Tehran, Iran.

出版信息

J Pharm Biomed Anal. 2018 Aug 5;157:1-9. doi: 10.1016/j.jpba.2018.05.004. Epub 2018 May 4.

Abstract

A simple and applied method based on ultrasound assisted-Ionic liquid trap-micro solid phase extraction (USA-ILT-μSPE) was demonstrated for preconcentration/separation of lead (Pb) in human blood and urine samples. By proposed method, the amine-functionalized bimodal mesoporous silica nanoparticles (NH-UVM) as solid phase sorbent was used for lead analysis in human biological samples at pH ≈ 7.0. After shaking/centrifuging of sample, the Pb (II) was extracted with NH-UVM without any chelating agents, trapped in ionic liquid phase and settled down in conical centrifuge tube as a residual solution [Pb→:NH-UVM]. Finally, the lead ions was back extracted from residual solution and determined by atom trap flame atomic absorption spectrometry (AT-FAAS). Under the optimal conditions, the linear range (LR), limit of detection (LOD) and preconcentration factor (PF) were obtained (10-950 μg L; 2.0-210 μg L), (2.8 μg L; 0.6 μg L) and (19.8; 99.7) for human blood and urine samples, respectively (% RSD < 1, intra-day). The reusability and adsorption capacity of the sorbent were also obtained 24 and 213.8 mg g, respectively. Validation of methodology was confirmed by certified reference materials (NIST, CRM).

摘要

一种基于超声辅助-离子液体捕集-微固相萃取(USA-ILT-μSPE)的简单实用方法被用于预浓缩/分离人血和尿样中的铅(Pb)。在所提出的方法中,胺功能化双模态介孔硅纳米粒子(NH-UVM)作为固相吸附剂,在 pH≈7.0 下用于人生物样品中的铅分析。在样品摇/离心后,无需任何螯合剂,Pb(II)即可用 NH-UVM 萃取,捕集在离子液相中,并在锥形离心管中沉降为残留溶液[Pb→:NH-UVM]。最后,从残留溶液中反萃取铅离子,并通过原子捕获火焰原子吸收光谱法(AT-FAAS)测定。在最佳条件下,得到了人血和尿样的线性范围(LR)、检测限(LOD)和预浓缩因子(PF)(10-950μg/L;2.0-210μg/L)、(2.8μg/L;0.6μg/L)和(19.8;99.7)(%RSD<1,日内)。还分别获得了 24 和 213.8mg/g 的吸附剂的可重复使用性和吸附容量。通过认证参考材料(NIST,CRM)验证了方法的验证。

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