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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.

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

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 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.

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.

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.

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.

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.

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.

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 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%.