Sensitive measurement of silver ions in environmental water samples integrating magnetic ion-imprinted solid phase extraction and carbon dot fluorescent sensor

Increasing use of silver in various fields has caused Ag^(+)pollution in water environment,taking great threats to people’s health.As a consequence,establishing rapid and reliable methods for sensitive determination of Ag^(+)is of great significance.Fluorescent(FL)sensors based on carbon dots(CDs),an excellent carbonaceous nanomaterial with strong and stable fluorescence,have absorbed extensive attentions in analysis of pollutants due to its advantages of carbon sources being readily available,low cost,easy operation and fast response.Moreover,ion-imprinting is a better way to increase the selectivity of the proposed method.Present work described an effective method for the sensitive measurement of silver ion in water samples in combination with magnetic ion-imprinted solid phase extraction and CDs based fluorescent sensor,which took full advantages of easy separation and high enrichment of magnetic solid phase extraction,high selectivity of ion-imprinting technology,and sensitivity and rapid response of fluorescent sensor from CDs.Sulfur-doped CDs derived from dithizone and magnetic ion-imprinted nanomaterial were prepared,and characterized with Fourier transform infrared spectroscopy and transmission electron microscope,etc.Magnetic Ag^(+)imprinted nanomaterial based solid phase extraction was employed for separating and enriching Ag^(+)from water samples.The significant parameters were optimized in detail.Under the optimal conditions,the proposed method provided good linearity in the range of 0.01-0.4μmol/L and low detection limit of 3 nmol/L.The reliability of the proposed method was validated with real water samples,and the results demonstrated that the proposed method was simple,robust,selective and sensitive detection tool for Ag^(+)in real water samples.

Preparation of Magnetic Molecularly Imprinted Polymers for Selective Isolation and Determination of Kaempferol and Protoapigenone in Macrothelypteris torresiana

Novel uniform-sized magnetic molecularly imprinted polymers （MMIPs） were synthe- sized for selective recognition of active antitumor ingredients of kaempferol （KMF） and protoapi- genone （PA） in Macrothelypteris torresiana （M. torresiana） by surface molecular imprinting tech- nique in this study. Super paramagnetic core-sheU nanoparticles （γ-MPS-SiO2@Fe3O4） were used as seeds, KMF as template molecule, acrylamide （AM） as functional monomer, and N, N＇-methylene bisacrylamide （BisAM） as cross-linker. The prepared MMIPs were characterized by X-ray diffraction （XRD）, Fourier transform infrared spectrum fiT/R）, transmission electron microscopy （TEM） and thermo-gravimetric analysis （TGA）, respectively. The recognition capacity of MMIPs was 2.436 times of non-imprinted polymers. The adsorption results based on kinetics and isotherm analysis were in accordance with the pseudo-second-order model （R2=0.9980） and the Langmuir adsorption model （R2=0.9944）. The value of E （6.742 kJ/mol） calculated from the Dubinin-Radushkevich isotherm model suggested that the physical adsorption via hydrogen-bonding might be predominant. The Scatchard plot showed a single line （R2=0.9172） and demonstrated the homogeneous recognition sites on MMIPs for KMF. The magnetic solid phase extraction （MSPE） based on MMIPs as sorbent was established for fast and selective enrichment of KMF and its structural analogue PA from the crude extract of M. torresiana and then KMF and PA were detected by HPLC-UV. The established method showed good performance and satisfactory results for real sample analysis. It also showed the feasi- bility of MMIPs for selective recognition of active structural analogues from complex herbal extracts.

Application of magnetic solid phase extraction in separation and enrichment of glycoproteins and glycopeptides

The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering substances makes the direct quantitative detection of low-abundance glycoproteins and glycopeptides in human body fluids one of the great challenges in analytical chemistry.Magnetic solid phase extraction(MSPE)has the advantages of easy preparation,low cost and good magnetic responsiveness.Magnetic adsorbents are the core of MSPE technology,and magnetic adsorbents based on different functional materials are widely used in the quantitative analysis of glycoproteins and glycopeptides in human body fluids,making it possible to analyze glycoproteins and glycopeptides with low abundance as well as multiple types,which provides a technical platform for screening and evaluating glycoproteins and glycopeptides in body fluids as disease biomarkers.In this paper,we focus on the recent advances in the application of MSPE technology and magnetic adsorbents for the separation and enrichment of glycoproteins and glycopeptides in human body fluids,and the future trends and application prospects in this field are also presented.

CoFe_(2)O_(4) decorated graphene/C_(18)-functionalized mesoporous silica nanocomposites prepared for magnetic enrichment and electrochemical detection of promethazine in beef

Promethazine(PHZ)is used as a sedative in veterinary medicine,and its residue can threaten the health of human.The electrochemical detection of PHZ is suitable method for application in the field.However,the traditional electroanalysis is difficult to perform directly in meat samples due to matrix interference.This work integrates magnetic solid-phase extraction and differential pulse voltammetry for highly sensitive and selective determination of PHZ in beef and beef liver for the first time.CoFe_(2)O_(4)/graphene coated with C_(18)-functionalized mesoporous silica(MG@mSiO_(2)-C_(18))is synthesized as dispersed magnetic adsorbent to extract PHZ.Magnetic glassy carbon electrode modified with nitrogen-doped hollow carbon microspheres(HCM)attracts the MG@mSiO_(2)-C_(18)with PHZ,and directly detects the PHZ without elution procedure.MG@mSiO_(2)-C_(18)can separate PHZ to avoid the interference of impurities on following detection,and also concentrate PHZ on magnetic electrode.Additionally,the electrode modification with HCM can amplify the electrochemical signal of PHZ.Finally,the integrated PHZ determination method exhibits a wide linear range from 0.08μmol/L to 300μmol/L with a low limit of detection of 9.8 nmol/L.The beef sample analysis presents excellent recovery,demonstrating that this protocol is promising for the rapid and onsite detection of PHZ in real meat samples。

Development of new solid phase extraction techniques in the last ten years

Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of solvent, high enrichment factor, high accuracy, etc. In recent years, a variety of new SPE methods such as molecularly imprinted solid phase extraction （MISPE）, magnetic solid phase extraction （MSPE）, solid phase micro-extraction （SPME）, etc., which are superior to the conventional SPE, have been developed and been widely applied to food, drugs, and environmental monitoring. In this paper, the basic principles and methods of SPE and its new applications in different areas are reviewed.