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Molecular imprinting technology (MIT) produces artificial binding sites with precise complementarity to substrates and thereby is capable of exquisite molecular recognition. Over five decades of evolution, it is predicted that the resulting host imprinted materials will overtake natural receptors for research and application purposes, but in practice, this has not yet been realized due to the unsustainability of their life cycles (i.e., precursors, creation, use, recycling, and end-of-life). To address this issue, greenificated molecularly imprinted polymers (GMIPs) are a new class of plastic antibodies that have approached sustainability by following one or more of the greenification principles, while also demonstrating more far-reaching applications compared to their natural counterparts. In this review, the most recent developments in the delicate design and advanced application of GMIPs in six fast-growing and emerging fields are surveyed, namely biomedicine/therapy, catalysis, energy harvesting/storage, nanoparticle detection, gas sensing/adsorption, and environmental remediation. In addition, their distinct features are highlighted, and the optimal means to utilize these features for attaining incredibly far-reaching applications are discussed. Importantly, the obscure technical challenges of the greenificated MIT are revealed, and conceivable solutions are offered. Lastly, several perspectives on future research directions are proposed.

Global concerns stem from the environmental crisis have compelled researchers to develop selective and sensitive methods for the identification and measurement of emerging pollutants in the environmental matrices. The cationic F-TMU-66

Advances in revolutionary technologies pose new challenges for human life; in response to them, global responsibility is pushing modern technologies toward greener pathways. Molecular imprinting technology (MIT) is a multidisciplinary mimic technology simulating the specific binding principle of enzymes to substrates or antigens to antibodies; along with its rapid progress and wide applications, MIT faces the challenge of complying with green sustainable development requirements. With the identification of environmental risks associated with unsustainable MIT, a new aspect of MIT, termed green MIT, has emerged and developed. However, so far, no clear definition has been provided to appraise green MIT. Herein, the implementation process of green chemistry in MIT is demonstrated and a mnemonic device in the form of an acronym, GREENIFICATION, is proposed to present the green MIT principles. The entire greenificated imprinting process is surveyed, including element choice, polymerization implementation, energy input, imprinting strategies, waste treatment, and recovery, as well as the impacts of these processes on operator health and the environment. Moreover, assistance of upgraded instrumentation in deploying greener goals is considered. Finally, future perspectives are presented to provide a more complete picture of the greenificated MIT road map and to pave the way for further development.

In this research work, molecularly imprinted biomembranes (MI-BMs) were fabricated by using the natural substance as a multifunctional monomer and methyl paraben as the template in a one-pot and gr...

The magnetic nanoparticles (MNPs) are applied as carriers for the efficient delivery of albendazole (ABZ) following its full characterization in terms of structure, morphology, size, and surface characteristics. The best composition and tunable properties for the achievement of more drug loading, controlled drug release, and delivery were optimized. A potential platform for anti-parasitic drug delivery was observed by uniform magnetic solid lipid NPs (MSLNPs) core/shell structure multifunctional mesoporous nano-capsules, which was composed of inorganic (Fe3O4) NPs as the core and stearic acid as the shell. This solid lipid NPs (SLNPs) and MSLNPs were identified and recognized by energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), Fourier-transform infrared spectroscopy (FTIR), and Dynamic light scattering (DLS) analyzer, which accordingly denote spherical particle morphology. The average particle sizes of SLNPs and MSLNPs were between 20 and 120 nm, depending on ultrasound irradiation, reagents concentration, and their order of addition. The ultrasound-prepared MSLNPs were homogeneously distributed with spherical shape and little agglomeration on SLNPs surface. Our in vitro release study demonstrated that 84.0% of ABZ was gradually released within 36 h. Moreover, in comparison to other strategies, the synthesis procedure presented here is more rapid and environment friendly and possesses high efficiency for ABZ delivery.

In this work, hydrophilic molecularly imprinted nanospheres (MINs) were synthesized via surface imprinting technology and subsequently utilized as dispersant sorbent in matrix solid phase dispersion (MSPD) for the extraction of rhodamine B (RhB) as the illogical food additive dye from different foodstuffs, followed by HPLC analysis. By considering hydrophilicity of target analyte, the sol-gel route was chosen for the preparation of MINs in aqueous media at mild conditions. Most importantly, both synthesis and extraction steps were designed and performed in the line of green chemistry and hazardous waste was eliminated to minimize detrimental impact on the operator health and the environment. The reputable experimental design methodology was adopted to assist the condition optimization of MSPD, which comprehends the significance of the factors and their interactions with the least experimental runs. Under optimized MINs-MSPD-HPLC conditions, the detection limit of RhB was down to 0.14 μg kg−1 and excellent linearity over the wide range of 0.5–10000 μg kg−1 was attained. Furthermore, endogenous RhB was found in the tested food samples with relative standard deviations (RSDs) of ≤4.6%, and satisfactory recoveries were from 83.6 to 96.9%. The simple green MINs-MSPD method holds great potential for determination of trace RhB in complicated solid/semi-solid samples, showing rapidity, accuracy and reliability.

A novel kind of cationic metal-organic framework(MOF) based mixed-matrix membrane(MMM) namely cationic MOF-MMM was firstly designed and used for simultaneous dispersive membrane extraction(DME) of six phenoxy carboxylic acid(PCA) herbicides from water samples followed by determination using ultrahigh-performance liquid chromatography tandem mass spectrometry. The cationic MOF-MMM was synthesized by soaking the zirconium-based MOFs in a polyvinylidene fluoride(PVDF) solution and further functionalization with quaternary amine groups, viz., UiO-66-NMe3+ MMM. The well-prepared UiO-66-NMe3+ MMM was characterized by FT-IR, SEM, XRD, XPS, NMR and etc. Several main variables influencing the MMM based DME efficiency were investigated and optimized in detail, such as dosage ratio of MOF/PVDF, solution pH, extraction time, coexistent anions and ionic strength. Electrostatic interactions dominated adsorption mechanism between anionic PCAs and cationic UiO-66-NMe3+ MMM, along with π π conjugation and cation-π bonding, leading to better adsorption performance. Low limits of detection in the range of 0.03–0.59 ng/L and satisfactory recoveries within 80.06–117.40 % for all the PCAs are a reliable witness to demonstrate supreme sensitivity and the applicability of the developed method. By relying on the obtained results, the present work implied cationic MOF-MMM based DME can be a versatile and worthy utility for extraction of pollutants from different water samples with high throughput.

Water compatible hollow porous molecularly imprinted nanospheres (HP-MINs) have been prepared for specific recognition and extraction of the blood pressure regulating drugs valsartan (VAL) and losartan (LOS). All synthetic steps were performed in aqueous medium and without consumption of organic solvents. The morphology and functionality of the materials were characterized by FT-IR, FE-SEM, and TEM techniques. The adsorption and selectivity experiments demonstrate that the HP-MINs possess a high binding capacity, fast kinetics, excellent water dispersibility and remarkable selectivity for VAL and LOS. The HP-MINs were utilized for dispersive solid phase extraction of VAL and LOS prior to their determination by HPLC-UV. Main variables and their interactions on extraction yield were optimized by multivariate analysis with least amount of experiments. Under optimized conditions, the method has a linear response in the 5–2000 μg L−1 concentration range of both VAL and LOS. The limits of detection are 1.5 μg L−1 for VAL and 1.4 μg L−1 for LOS.

This study is devoted on Allura Red as food colorant preconcentration and determination in beverage, fruit juice and drink water samples is based on usage of Mn- and Cu- @ ZnS-NPs-AC as new sorbent for ultrasound-assisted-dispersive solid-phase microextraction (UA-DSPME) combined with ultraviolet–visible spectrophotometric based method (UV–Vis). Contribution of volume of eluent, pH, sorbent mass and sonication time on response following conduction of 28 experiments were optimized and investigated while their significantly justified according to p-value. Values of “Prob > F” less than 0.0500 is proportional with their significant influence on recovery of analyte. Under the optimum conditions 0.14 mL of THF; pH of 2.5; 8 mg of sorbent and 3 min sonication time guide and help achievement of limit of quantification (LOQ) and limit of detection (LOD) of 6.08 and 20.26 ng mL−1, respectively. The accuracy of method was validated according to calculation of recovery following spiking 400 and 600 ng mL−1 to blank solution and recovery as more reliable indication of accuracy 93.41 and 102.17% recoveries with RSD

The objective of this study was to develop a simple, sensitive and selective procedure for the preconcentration and determination of quercetin residues in Apium graveolens, Brassica oleracea, Spinacia oleracea, watercress, onion, and apple matrices. This novel method was developed on the basis of the dispersive-micro-solid phase extraction (D-μ-SPE) procedure based on a core–shell magnetic molecularly imprinted polymer (MMIP) in combination with high-performance liquid chromatography-ultraviolet (HPLC-UV). Variables affecting the quercetin extraction efficiency included pH, MIP dose, extraction contact time, elution organic solvent, and volume of organic solvent and were evaluated by the experimental central composite design (CCD). The obtained optimal parameters were as follows: pH (3.5), sorbent (12 mg), elution organic solvent and solvent volume (methanol, 0.2 mL), and elution time (22.0 min, without adding salt). The calibration curve was linear in the concentration range of 0.6–5500 μg L−1 with the lower limits of detection found in the range of 0.113–0.117 μg L−1, thereby revealing the high-sensitivity and -selectivity properties. The combination of D-μ-SPE and HPLC-UV could provide a method for the recovery of the analyte in various matrices at 22 min contact time with good reusability and excellent recoveries at four concentration levels (50, 100, 500, and 1000 μg L−1), ranging between 95.44 and 106.89% (relative standard deviation

In this work, a fast, sensitive, inexpensive and environment-friendly dispersive liquid–liquid microextraction (DLLME) technique was developed based on solidification of floating organic drops (SFOD) for the preconcentration of quercetin followed by HPLC-UV. The parameters affecting the extraction efficiency (the type of extractant and disperser solvents and their volume, sample pH, concentration of salt, and sonication time) in the DLLME-SFOD-HPLC-UV method were studied and optimized with the aid of experimental designs. The optimum conditions found were as follows: extractant solvent type and amount, 0.25 mL of dodecanol, disperser solvent type and amount, 0.70 mL of acetonitrile, pH 5.0, extraction time of 0.5 min, and no need of adding salt. Under the optimal conditions, a good linearity in the range of 0.8–3500 μg L−1 was reached; furthermore, our proposed method had a reasonable reproducibility (RSD% 1.94–5.20), repeatability (RSD% 1.01–2.82), and recovery (96.65–106.76%). In addition, a low LOD (0.149–0.165 μg L−1), high enrichment factor, and very little extraction time were attained for different aqueous matrices (Nasturtium officinale, Apium graveolens, Brassica oleracea var. sabellica, Spinacia oleracea and food samples).

The present study attempted to develop a fast and sensitive ultrasound-assisted-dispersive-micro-solid phase extraction (UA-D-μ-SPE) method for the separation and preconcentration of albendazole (ABZ) from plasma and urine samples, using a molecularly imprinted polymer (MIP) coupled with high-performance liquid chromatography-UV (HPLC-UV). An MIP was selected as a sorbent, and the main factors viz. pH, MIP mass, sonication time, and eluent volume were optimized using CCD-RSM (central composite design-response surface methodology). Under the optimum conditions, the method showed the detection limit of 1.46, quantification of 4.86, and linear range of 10.0–6000.0 ng mL−1. The relative standard deviation and the relative recoveries of ABZ from spiked plasma and urine samples at five concentration levels (20, 50, 100, 500, and 1000 ng mL−1) were in the ranges of 1.43–5.21% and 92.48–101.40%, respectively. The kinetic sorption curve indicated that six min was sufficient to achieve sorption equilibrium for MIPNPs (MIP nanoparticles). The maximum sorption capacity was 34.9 mg g−1. All these results strongly support the high efficiency, selectivity, and sensitivity of the developed method for determining ABZ in plasma and urine samples.

In present work, facile method is developed for determination of colchicine in human plasma sample, autumn and spring root of colchicium extracts by ultrasound assisted dispersive magnetic solid phase microextraction followed by HPLC-UV method (UAD-MSPME-HPLC-UV). Magnetic (Fe2O4-nanoparticles) metal organic framework-5, (MOF-5(Zn)-Fe2O4NPs) was synthesized by dispersing MOF-5 and Fe(NO3)3.9H2O in ethylene glycol (as capping agent) and NaOH (pH adjustment agent) by hydrothermal method. The prepared sorbent was characterized via XRD and SEM analysis and applied as magnetic solid phase in UAD-MSPME-HPLC-UV method. In this method, colchicine molecules were sorbed on MOF-5(Zn)-Fe2O4NPs sorbent by various mechanisms like ion exchange, hydrogen bonding and electrostatic, ᴨ-ᴨ, hard-hard and dipole-ion interaction followed by exposing sonication waves as incremental mass transfer agent and then the sorbent was separated from the sample matrix by an external magnetic fields. Subsequently, accumulated colchicine were eluted by small volume of desorption organic solvent. Influence of operational variables such as MOF-5(Zn)-Fe2O4NPs mass, volume of extracting solvent and sonication time on response property (recovery) were studied and optimized by central composite design (CCD) combined with desirability function (DF) approach. Under optimum condition, the method has wide linear calibration rang (0.5-1700ngmL-1) with reasonable detection limit (0.13ngmL-1) and R2=0.9971. Finally, the UAD-MSPME-HPLC-UV method was successfully applied for determination of colchicine autumn and spring root of colchicium extracts and plasma samples.

It is still challenging to sensitively detect protein biomarkers via surface-enhanced Raman scattering (SERS) technique owing to their low Raman activity. SERS tag-based immunoassay is usually applied; however, it is laborious and needs specific antibodies. Herein, an ultrasensitive and universal “Raman indicator” sensing strategy is proposed for protein biomarkers, with the aid of a glass capillary-based molecularly imprinted SERS sensor. The sensor consists of an inner SERS substrate layer for signal enhancement and an outer mussel-inspired polydopamine imprinted layer as a recognition element. Imprinted cavities have two missions: first, selectively capturing the target protein, and second, the only passageway of Raman indicator to access SERS substrate. Specific protein recognition means filling imprinted cavities and blocking Raman indicator flow. Thus, the quantity of captured protein can be reflected by the signal decrease of ultra-Raman active indicator molecule. The capillary sensor exhibited specific and reproducible detection at the level down to 4.1 × 10−3 μg L−1, for trypsin enzyme in as-received biological samples without sample preparation. The generality of the mechanism is confirmed by using three different protein models. This platform provides a facile, fast and general route for sensitive SERS detection of Raman inactive biomacromolecules, which offers great promising utility for in situ and fast point-of-care practical bioassay.

Separation and detection of residual drug in biological fluids has directly related to human health in term of their beneficial or side effects. In biological fluid samples (complex matrix which containing drug at very low level) conduction of preliminary efficient technique as good choice for pre-concentration and clean-up of real sample before their instrumental analysis is highly recommended. In this result technique, based on nano-structure material which poses higher available surface area and larger member of reactive sites led to significant improvement in characteristic performance of analytical method. This paper focused on the synthesis and application of novel nano-sorbent for pre-concentration and extraction of atorvastatin (AT) from different biological fluids. Influence of various variables including sorbent dosage, eluent volume and sonication time on present method response was studied and optimized by central composite design under response surface methodology and accordingly an acceptable calibration curves over wide linear ranges (0.3–2000 μg L−1) with high coefficient of determination higher than 0.999 strongly confirm high applicability of present method for quantification of analyte while limit of detection and quantification in plasma sample were 0.0608 and 0.2033 μg L−1, respectively.

In the present paper, one-pot green syntheses of novel hydrophilic and superparamagnetic molecularly imprinted polymers (MMIPs) for the cleanup and extraction of hydrochlorothiazide (HCT) in human urine are described. The MMIPs were prepared via a sol–gel process using Fe3O4 magnetite as a magnetic component, HCT as a template, tetraethyl orthosilicate (TEOS) as the cross-linker, and 3-aminopropyl trimethoxysilane (APTMS) as the functionalized monomer, which could simplify the imprinting process. During the synthesis process, a surfactant was especially used to graft the silica-imprinted nanoparticles. The key step of this research is mild working temperature without consuming any organic solvent during the synthesis of MMIPs in addition to its ability for efficient and highly selective enrichment of HCT in complicated human urine. The morphology, structure, and magnetic properties of the MMIPs were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier tra...

The authors describe the preparation of molecularly imprinted nanoparticles (MINPs) for the solid phase extraction of hippuric acid (HA). The MINPs consists of a water-compatible organic-inorganic silica composite which was obtained from a functionalized silica by the sol-gel method. HA acted as the template, 3-aminopropyl trimethoxysilane as the functional monomer, and tetraethoxysilane as the crosslinker. Subsequently, methacryloxypropyltrimethoxysilane was used as a coupling agent to deposit a hydrophilic acrylamide coating onto the surface of the MINPs. The morphology and structure of the resulting restricted access material (referred to as RAM-MINP) were characterized by scanning electron microscopy, transmission electron microscopy and Fourier transform infrared spectroscopy. Solid phase extraction of HA was accomplished by passing urine samples through a RAM-MINP-packed SPE cartridge. Following elution, HA was quantified by HPLC using UV detection at 228 nm. The effects of sample pH, amount of sorbent and eluent and washing solvent volumes were optimized by experimental design methodology under response surface methodology. Under optimized conditions, the mean extraction efficiency of HA from spiked samples is adequately repeatable, with relative standard deviations of

In this work molecular imprinted nanoparticles (MINPs) was synthesized and applied for ultrasonic assisted solid phase extraction of celecoxib (CEL) from human plasma sample following its combination by HPLC-UV. The MINPs were prepared in a non-covalent approach using methacrylic acid as monomer, CEL as template, ethylene glycol dimethacrylate as cross-linker, and 2,2-azobisisobutyronitrile (AIBN) as the initiator of polymerization. pH, volume of rinsing and eluent solvent and amount of sorbent influence on response were investigated using factorial experimental design, while optimum point was achieved and set as 250mg sorbent, pH 7.0, 1.5mL washing solvent and 2mL eluent by analysis of results according to design expert (DX) software. At above specified conditions, CEL in human plasma with complicated matrices with acceptable high recoveries (96%) and RSD% lower than 10% was quantified and estimated. The proposed MISPE-HPLC-UV method has linear responses among peak area and concentrations of CEL in the range of 0.2-2000μgL(-1), with regression coefficient of 0.98. The limit of detection (LOD) and quantification (LOQ) based on three and ten times of the noise of HPLC peaks correspond to blank solution were 0.08 and 0.18μgL(-1), respectively.

A novel technique was applied for the synthesis of dummy molecularly imprinted silica nanoparticles (DMISNPs). DMISNPs were characterized by Fourier transmission infrared spectrometry, scanning electron microscopy and transmission electron microscope. The material was used as dispersant for the analysis of biscuit and bread samples using matrix solid phase dispersion (MSPD). Of advantages of such approach may be counted as the simplicity of synthesis procedure, low consumption of organic solvent, mild working temperature during the synthesis, high binding capacity and affinity. The effect of various parameters such as sample-to-dispersant ratio and eluents volume on extraction recovery was investigated and optimized by central composite design under response surface methodology. It was proven that the proposed dispersant leads to high affinity toward acrylamide even in complicated matrices. Quantification of the acrylamide was carried out by high performance liquid chromatography with UV detection (HPLC-UV).

This paper reports a new variant of sample clean-up procedure based on miniaturized matrix solid phase dispersion (MSPD) combining with water compatible magnetic molecularly imprinted polymers (MMIP) for preconcentration of melamine from milk samples prior high-performance liquid chromatography with UV detection. By employing MMIP as dispersant sorbent matrix interferences could be eliminated completely and the column packing step was interestingly omitted that decreasing in glassware expenditure, labor effort and extraction time which cause improvement of the method performance. In order to investigate the functionality, morphology and magnetic properties of the prepared MMIP, it was fully characterized by FT-IR, VSM, SEM, and TEM. Multivariate optimization was applied as a versatile statistical approach for evaluating the influence of the main variables and their interactions on extraction efficiency. Under optimized conditions, the proposed method exhibited a wide linear response in the concentration range of 250.0–5000.0 μg L−1, satisfactory recoveries for all samples (86.6% ≤), and supreme repeatability (RSD less than 6.3%) were achieved as well. The low limit of detection close to 67.0 μg L−1 implied high ability of proposed method for isolation of melamine from complicate milk sample. These befitting results demonstrated that the developed method is unique in terms of the facility, rapidly and least solvent consumption as well as accurate analysis of melamine at trace levels.

In this work, novel dummy molecularly imprinted polymers (DMIP) with propanamide as a dummy template molecule were prepared based on a green synthesis strategy of less consumption of hazardous/organic reagents and at mild conditions for magnetic solid-phase extraction (MSPE) of acrylamide in biscuit samples, followed by high performance liquid chromatography (HPLC) determination. The resultant DMIP was well characterized by FT-IR, SEM, TEM and VSM, exhibiting uniform nanoscale coreshell structure and good magnetic property in favor of simple rapid separation. Several main variables influencing MSPE efficiency were investigated, including DMIP dosage, sample solution pH, extraction time and desorption solvent; central composite design (CCD) and response surface methodology (RSM) were employed to assist in the MSPE condition optimization with rapidity and reliability. Under optimized conditions, excellent linearity for acrylamide was obtained in the range of 5.0–5000.0 µg kg−1, and low detection and quantification limits were 1.3 µg kg−1 and 4.4 µg kg−1, respectively. The method recoveries at five spiked concentrations were found within 86.0–98.3% with relative standard deviations (RSDs) of 1.2–4.1%. Furthermore, endogenous acrylamide was detected in five different biscuit samples and the RSDs values were lower than 3.3%. The present study suggested promising perspectives of water-compatible eco-friendly DMIP based MSPE-HPLC method for highly effective sample pretreatment and targeted analytes determination in complicated matrices.

Molecular imprinting-based solid-phase extraction (MI-SPE) has been in the spotlight to improve the recognition selectivity and detection sensitivity. MI-SPE provides a powerful tool for chemo/bioanalysis in complex matrices and meanwhile, benefits from distinguished advantages such as easy operation, high throughput, low cost, high selectivity and durability. This review proposed the recent advances in molecular imprinting concerning novel preparation strategies of molecularly imprinted polymers (MIPs) and typical applications of MI-SPE. Preparation strategies are highlighted by dividing into ten sections mainly including dummy imprinting, multi-template imprinting, surface imprinting, water-compatible imprinting, restricted access material combining imprinting etc.; each section provides the descriptions about what restrictions led to the emergence of any strategy, strengths/weaknesses of every strategy and universal applications of upgraded MIPs in various SPE modes prior to chromatographic analysis. The potential of MIPs for implementation in routine laboratory activities and scale-up is expected, and finally remaining challenges and future perspectives are proposed.

A molecularly imprinted polymer was selectively applied for solid-phase extraction and diazinon residues enrichment before high-performance liquid chromatography. Diazinon was thermally copolymerized with Fe3O4@polyethyleneglycol nanoparticles, methacrylic acid (functional monomer), 2-hydroxyethyl methacrylate (co-monomer), and ethylene glycol dimethacrylate (cross-linking monomer) in the presence of acetonitrile (porogen) and 2,2-azobisisobutyronitrile (initiator). Then, the imprinted diazinon was reproducibly eluted with methanol/acetic acid (9:1, v/v). The sorbent particles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. The comprehensive study of variables through experimental design showed that the maximum performance was achieved under these conditions: pH 7, 10 mL sample volume, 15 mg sorbent, 10 min vortex time, 5 min ultrasonic time, 200 μL methanol/acetic acid (9:1, v/v) as eluent, and 5 min desorption time. Under optimized conditions, the molecularly imprinted polymer solid-phase extraction method demonstrated a linear range (0.02–5 g/mL), a correlation coefficient of 0.997, and 0.005 g/mL detection limit.

A novel green synthesis strategy was proposed for preparation of multitemplate molecularly imprinted biopolymers (mt-MIBP) in aqueous media with less consumption of organic solvents, which were subsequently used as sorbents of ultrasound-assisted dispersive solid-phase extraction (d-SPE) for simultaneous recognition and efficient separation of B-family vitamins in juice samples, followed by high performance liquid chromatography (HPLC) determination. The obtained mt-MIBP was fully characterized by SEM, FT-IR, TEM, and BET. It offered high binding capacity, good selectivity, and fast dynamics toward all the templates. Involved parameters in the d-SPE efficiency such as mt-MIBP mass, sonication time, and eluting/washing solvents' types and volumes were concurrently investigated by central composite design with rapidity and reliability. Under the optimum conditions, the developed mt-MIBP-d-SPE-HPLC method exhibited wide linear range, low limits of detection and quantification (LOQs) within 1.2-5.5 μg L-1 and 4.0-18.4 μg L-1, respectively, and appropriate repeatability (relative standard deviation values below 4.2%, n = 4). The high selectivity of this method makes it suitable for successful monitoring of vitamins in juice samples with satisfactory recoveries of 75.8-92.7%, 81.1-92.5%, and 84.7-93.8% for vitamins riboflavin (B2), nicotinamide (B3), and pyridoxine (B6), respectively. The present study implied highly promising perspectives of water-compatible eco-friendly mt-MIBP for highly effective multiresidue analysis in complicated matrixes.

In present work, facile method is developed for determination of colchicine in human plasma sample, autumn and spring root of colchicium extracts by ultrasound assisted dispersive magnetic solid phase microextraction followed by HPLC-UV method (UAD-MSPME-HPLC-UV). Magnetic (Fe

In the present work, hollow porous molecularly imprinted polymer (HPMIP) was prepared via adopting a sacrificial support approach using glibenclamide (GB) as template, methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate as cross-linker (EGDMA) and mesoporous MCM-48 nanospheres as support. Owing to a short thickness of the foresaid HPMIP, a suitable steric structure was readily available that lead to fast and effective mass transfer of target analyte to sorbent and consequently supply high binding capacity. After ultrasonic-assisted dispersive solid phase extraction of urine sample, the analyte of interest was quantitatively pre-concentrated and determined by high performance liquid chromatography-ultraviolet detection (HPLC-UV). Influence of factors affecting the extraction efficiency such as sonication time, sample pH, sorbent dosage, and volumes of eluent and washing agents as well as their significant interactions were simultaneously optimized by experimental design methodology. Under optimized conditions, present method has linear response over concentration range of 10.0-3000.0μgL-1 in human urine samples with a satisfactory detection limit close to 3.5μgL-1. The inter-day precisions of the current method (coefficient of variation) are lower than 5%, while recoveries are more than 89.5%.

Ultrasound-assisted dispersive solid phase microextraction followed by UV–Vis spectrophotometry (UA-DSPME UV–Vis) was designed for the extraction and preconcentration of Carbaryl using nano-sized molecularly-imprinted polymer (MIP-NP). Nano-sized Carbaryl-imprinted polymer was characterized by scanning electron microscopy. A preliminary Plackett–Burman design was applied for screening. Subsequently, central composite design under response surface methodology was used to investigate and model the Carbaryl adsorption as response as well as to optimize this response versus variables such as Carbaryl MIP-NP mass, sonication time, temperature, eluent volume, pH and vortex time. At optimum experimental conditions, UAMSPE-UV–Vis exhibited a linear range of 0.1–1.2 mg L−1. The enhancement and preconcentration factors were obtained to be 30.6 and 25.0, respectively, for the extraction of Carbaryl by MIP-NP. In addition, the values of 0.033 and 0.11 mg L−1 were obtained for limit of detection and limit of quantification, respectively. The value of 4.3% determined for relative standard deviation for the separation and preconcentration of Carbaryl after 5 repetitions shows the acceptable repeatability of the process. Finally, the developed method was successfully applied for the determination of Carbaryl in water samples.

In this research, a facile and selective method was described to extract l -cysteine ( l -Cys), an essential α-amino acid for anti-ageing playing an important role in human health, from human blood plasma sample. The importance of this research was the mild and time-consuming synthesis of zinc organic polymer (Zn-MOP) as an adsorbent and evaluation of its ability for efficient enrichment of l -Cys by ultrasound-assisted dispersive micro solid-phase extraction (UA-DMSPE) method. The structure of Zn-MOP was investigated by FT-IR, XRD and SEM. Analysis of variance (ANOVA) was applied for the experimental data to reach the best optimum conditions. The quantification of l -Cys was carried out by high performance liquid chromatography with UV detection set at λ = 230 nm. The calibration graph showed reasonable linear responses towards l -Cys concentrations in the range of 4.0–1000 μg/L (r 2 = 0.999) with low limit of detection (0.76 μg/L, S/N = 3) and RSD ≤ 2.18 (n = 3). The results revealed the applicability and high performance of this novel strategy in detecting trace l -Cys by Zn-MOP in complicated matrices.

A novel strategy was presented for the synthesis and application of functionalized silica monolithic as artificial receptor of gallic acid at micro-pipette tip. A sol–gel process was used to prepare the sorbent. In this in-situ polymerization reaction, tetraethyl orthosilicate (TEOS), 3-aminopropyl trimethoxysilane (APTMS), gallic acid and thiourea were used, respectively, as cross-linker, functionalized monomer, template and precursor to make crack-free and non-fragile structure. Such durable and inexpensive in-situ monolithic was successfully employed as useful tool for highly efficient extraction of gallic acid from orange juice samples. The effective parameters in extraction recovery were investigated and optimum conditions were obtained using experimental design methodology. Applying HPLC-UV for separation quantification at optimal conditions, the gallic acid was efficiently extracted without significant matrix interference. Good linearity for gallic acid in the range of 0.02–5.0 mg L−1 with correlation coefficients of R2 > 0.999 revealed well applicability of the method for trace analysis.

Separation and detection of residual drug in biological fluids has directly related to human health in term of their beneficial or side effects. In biological fluid samples (complex matrix which containing drug at very low level) conduction of preliminary efficient technique as good choice for pre-concentration and clean-up of real sample before their instrumental analysis is highly recommended. In this result technique, based on nano-structure material which poses higher available surface area and larger member of reactive sites led to significant improvement in characteristic performance of analytical method. This paper focused on the synthesis and application of novel nano-sorbent for pre-concentration and extraction of atorvastatin (AT) from different biological fluids. Influence of various variables including sorbent dosage, eluent volume and sonication time on present method response was studied and optimized by central composite design under response surface methodology and accordingly an acceptable calibration curves over wide linear ranges (0.3-2000μgL

A selective and rapid method was developed for quantification of curcumin in human plasma and food samples using molecularly imprinted magnetic multiwalled carbon nanotubes (MMWCNTs) which was characterized with EDX and FESEM. The role of sorbent mass, volume of eluent and sonication time on response in solid phase microextraction procedure were optimized by central composite design (CCD) combined with response surface methodology (RSM) using Statistica. Preliminary experiments reveal that among different solvents, methanol:dimethyl sulfoxide (4:1V/V) led to efficient and quantitative elution of analyte. A reversed-phase high performance liquid chromatographic technique with UV detection (HPLC-UV) was applied for detection of curcumin content. The assay procedure involves chromatographic separation on analytical Nucleosil C18 column (250×4.6mm I.D., 5μm particle size) at ambient temperature with acetonitrile-water adjusted at pH=4.0 (20:80, v/v) as mobile phase at flow rate of 1.0mLmin-1, while UV detector was set at 420nm. Under optimized conditions, the method demonstrated linear calibration curve with good detection limit (0.028ngmL-1) and R2=0.9983. The proposed method was successfully applied to biological fluid and food samples including ginger powder, curry powder, and turmeric powder.

A novel pipette-tip based on nano-sized dummy molecularly imprinted polymer (PT-DMIP) assisted by ultrasonication for the effective enrichment and analysis of prednisolone from urine samples was developed. The PT-DMIP cartridge was prepared by packing the dummy molecularly imprinted polymer at the tip of the micropipette. The polymerization used betamethasone (BM) as the dummy template, 3-aminopropyltrimethoxysilane (APTMS) as the functionalized monomer, tetraethyl orthosilicate (TEOS) as the cross-linker and aluminum ion (Al(3+)) as a dopant to produce Lewis acid sites in the silica matrix for metal coordinative interactions with the analyte. Compared to conventional solid phase extraction (SPE), the PT-DMIP is cost-effective, fast, and easy to handle, while the system is very approachable and reduces the consumption of toxic organic solvent. HPLC-UV analysis revealed successful applicability of the sorbent for highly efficient extraction of perdnisolone from urine matrices. The extraction recovery was investigated and optimum conditions were obtained using central composite design. Good linearity for prednisolone in the range of 0.22-220μgL(-1) with regression coefficients of 0.99 reveals high applicability of the method for trace analysis. Under the optimized conditions, the recoveries are 89.0-96.1 with relative standard deviations (RSD) of less than 9.0%.

This study discusses a novel and simple method for the preparation of magnetic dummy molecularly imprinted nanoparticles (MDMINPs). Firstly, Fe3O4 magnetic nanoparticles (MNPs) were synthesized as a magnetic component. Subsequently, MDMINPs were constructed via the sol-gel strategy using APTMS as the functional monomer. Urethane was considered as dummy template to avoid residual template and TEOS as the cross linker. The prepared MDMINPs were used for the pre-concentration of acrylamide from potato chips. Quantification was carried out by high performance liquid chromatography with UV detection (HPLC-UV). The impact of influential variables such as pH, amount of sorbent, sonication time and eluent volume were well investigated and optimized using a central composite design. The particles had excellent magnetic property and high selectivity to the targeted molecule. In optimized conditions, the recovery ranged from 94.0% to 98.0% with the detection limit of 0.35µgkg(-1).

This paper report a novel strategy for synthesis and application of CuS@ZnS@Fe3O4-CNTs composite which has great potentials as artificial receptor for tartrazine trapping due to its ultrahigh surface area and functionality which is related to application of electrochemical route. A durable and economical pipette-tip CuS@ZnS@Fe3O4-CNTs nano-composite miniaturized solid phase extraction coupled with UV-Vis spectrophotometry was developed for clean-up and determination of tartrazine from various water samples. Undoubtedly, presence of mild-intensity/frequency ultrasound irradiation played a key role for reducing consumption of eluent volume by broking hydrogen bonds between retained analyte and sorbent. The influence of factors including pH, sorbent dosage, sonication time and eluent volume were investigated and optimum conditions were obtained using experimental design methodology. Under optimized conditions, good extraction efficiencies for the analyte were obtained with no matrix interference in the subsequent UV-Vis. Good linearity for tartrazine in the range of 20-5000 ng mL-1 with correlation coefficients of R2 ≥ 0.99 and low detection limit close to 4.76 ng mL-1 reveals high applicability of method for trace analysis.

Well-designed metal organic materials (MOMs) were synthesized and applied for pre-concentration and determination of sodium valproate (Na-VP) from biological samples, bound to the copper complex of 1,4-phenylenedioxydiacetic acid under mild conditions. The channels of this sorbent provide high efficiency and also selectivity. The MOMs were structurally characterized using Fourier transform infrared and energy-dispersive X-ray spectroscopies, scanning electron microscopy and X-ray diffraction, and they were found to have suitable features for quantification of Na-VP using HPLC coupled with UV detection at λ = 215 nm. Moreover, the rate of adsorption is improved by ultrasonic power and the experimental data are best fitted according to Freundlich adsorption isotherm. According to the central composite design, the best experimental conditions are 280.0 μl, 3.0 min and 17.0 mg for volume of eluent, sonication time and sorbent mass respectively. Calibration plots show linear responses towards Na-VP concentrations (0.4–18.0 μg ml−1), satisfactory limit of detection (0.06 μg ml−1, S/N = 3) and reasonable enrichment factor (70.58). The coefficient of variation values of both inter- and intra-day analyses were less than 4.0%, indicating a candidate method for the determination of Na-VP in human plasma with reasonable recovery and efficiency.