Acid-base reaction-based dispersive solid phase extraction of favipiravir using biotin from biological samples prior to capillary electrophoresis analysis.

In this study, an acid-base reaction-based dispersive solid-phase extraction method was developed for the extraction of favipiravir from deionized water, plasma and urine samples prior to its determination using a capillary electrophoresis-diode array detector. The target analyte was extracted from the samples using biotin as a green adsorbent. To reach this goal, the pH of the solution was first adjusted to 9.0 (using borate buffer), and the ionic strength of the solution was enhanced by adding sodium chloride (2.5%, w/v). Thereafter, an appropriate amount of biotin was dissolved in the solution and a homogenous phase was obtained. By adding hydrochloric acid to the solution, an acid-base reaction occurs via protonation of biotin, which decreases its solubility. During this procedure, the analyte was adsorbed onto the tiny particles of the produced adsorbent dispersed into the solution. The resulting mixture was sonicated to facilitate the adsorption of the analyte onto the adsorbent surface. After the collection of biotin particles through centrifugation, the analyte was eluted using acetonitrile and then used in the determination stage. Under the optimal extraction conditions, the calibration curve was linear from 250 to 3000 ng mL-1 with a coefficient of determination of 0.9968. Low limit of detection, and quantification, good repeatability on the same day and different days (relative standard deviation ≤ 8.2%), and acceptable extraction recovery were accessed. The applicability of the method was examined by performing it on spiked plasma and urine samples, and its performance was verified.

Quantification of Arbutin and its degradation products, hydroquinone and p-Benzoquinone, in hyperpigmentation topical formulation: Effect of extraction procedure and interference assessment.

The utilization of Hydroquinone (HQ) in over-the-counter skincare items is subject to restrictions. Consequently, Arbutin (AR) serves as a reliable alternative for addressing hyperpigmentation in non-prescription topical formulations. Nevertheless, AR undergoes decomposition into HQ and p-Benzoquinone (BZ) when exposed to temperature stress, ultraviolet light, or dilution in an acidic environment, all of which can induce skin toxicity. The intention of this paper is to investigate the effect of extraction procedure on the conversion of AR to HQ and or BZ and to evaluate kinetics of AR hydrolysis to HQ. Meanwhile this study aims to evaluate AR and BZ interference with the United States Pharmacopoeia (USP) identification and assessment method for HQ Hydrolytic stress during extraction conditions underwent optimization through systematic screening tests. Subsequent assessment of the residual drug and its degradation products were achieved by HPLC method. The resulting data were meticulously fitted to various kinetic models. To analyze the potential interference of AR in HQ measurement using USP method, the standard concentrations of AR and HQ were analyzed through UV-VIS spectrophotometry. For enhanced certainty, a validated HPLC method analysis was also conducted. Notably, the acid hydrolysis of AR exhibited independence from its initial concentration. So, the hydrolytic degradation of AR exhibited a Zero-order kinetic profile. Furthermore, the proven interference of AR in the UV-VIS spectrophotometry method was identified within the context of the USP method. This study successfully utilized an adopted HPLC method for the concurrent quantification of AR, HQ, and BZ. The potential interference of AR in the UV-VIS spectrophotometric assay for HQ may lead to false results especially for regulatory purposes.

Development of dispersive solid phase extraction based on magnetic metal organic framework for the extraction of sunitinib in biological samples and its determination by high performance liquid chromatography-tandem mass spectrometry.

Herein, a simple, sensitive, and reliable dispersive solid phase extraction was reported for the efficient extraction of sunitinib from biological samples. To facilitate the extraction of the desired analyte from urine and plasma samples, magnetic MIL-101Cr (NH2) @SiO2 @ NiFe2O4 was synthesized by a hydrothermal method and applied as an effective sorbent during the extraction process. After adsorption of the drug using 10 mg of MIL-101Cr (NH2) @ SiO2 @ NiFe2O4 nanoparticles through vortexing (1 min), the sorbent was separatedfrom the sample solution using a magnet. To eluate the drug, the sorbent containing the sunitinib was contacted with 100 µL dimethylformamide. The eluent was analyzed by high performance liquid chromatography-tandem mass spectrometry. Reasonable validation data consisting of low limits of detection (0.14, 0.35, and 0.70 ng mL-1 in deionized water, plasma, and urine) and quantification (0.48, 1.2, and 2.4 ng mL-1 in deionized water, plasma, and urine, respectively), a wide linear range of the calibration curve (0.48-200, 1.2-200, and 2.4-100 ng mL-1 in deionized water, plasma, and urine, respectively) good extraction recovery (76 %), and low relative standard deviations for inter- and intra-day precisions (6.9 %) were obtained by the method. Eventually, the proposed procedure was effectively implemented on both plasma and urine samples, yielding successful outcomes.

In-situ formation of CO2-incorportaed solid sorbent for dispersive solid phase extraction of phenolic compounds from water and wastewater samples prior to gas chromatography-flame ionization detector.

BACKGROUND: Herein, a new extraction procedure based on in-situ formation of carbon dioxide-incorporated solid sorbent was introduced for dispersive solid phase extraction of phenolic compounds from aqueous samples. In this study, incorporation of carbon dioxide into the structure of a diamine led to the formation of a solid compound in the sample solution that adsorbed the analytes. RESULTS: The sample solution was mixed with isophorone diamine and placed under carbon dioxide stream. By doing so, isophorone diamine reacted with carbon dioxide and produced a carbamic acid analogue. It was dispersed into the sample solution as tiny particles that adsorbed the analytes. The adsorbed analytes were eluted by a volatile organic solvent and concentrated more by the vaporization of the eluate. The extraction procedure was done at low temperature to limit the releasing carbon dioxide from the produced compound. To obtain the reliable results, the method was validated and the obtained limits of detection and quantification were in the ranges of 0.29-41 and 0.96-1.3 ng/mL, respectively. Acceptable relative standard deviation (≤7.3%) and coefficient of determination (≥0.994) values confirmed the method repeatability and linearity. High enrichment factors (410-435) and extraction recoveries (82-87%) were attained with the introduced method. SIGNIFICANCE AND NOVELTY: In this work, a chemical reaction was done between isophorone diamine and carbon dioxide in solution. The produced product (sorbent) was insoluble in solution and dispersed in whole parts of the solution as tiny particles. A high contact area between the sorbent and analytes provided high extraction efficiency for the analytes. The method was successful utilized in determining target analytes in real samples and the matrix effect of the samples had no important effect on the obtained results.

Efficient and straightforward spectrophotometric analysis of 5-hydroxymethylfurfural (HMF) using citrate@Fe3O4 nanoparticles as an adsorbent.

In this study, we developed a spectrophotometry method for the analysis of 5-hydroxymethylfurfuraldehyde (HMF) in pharmaceutical formulations using citrate@Fe3O4 adsorbent. As bare magnetite (Fe3O4) has certain limitations, such as aggregation and oxidation, surface modifications are commonly used to improve its properties. We successfully coated Fe3O4 with sodium citrate to create a magnetic adsorbent for isolating HMF from samples. We confirmed the successful surface coating of Fe3O4 with citrate using Fourier Transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Zeta potential, and scanning electron microscopy (SEM). The high adsorption capacity of citrate@Fe3O4 is due to the abundance of carboxyl and hydroxyl groups on the surface of the adsorbent, making it ideal for HMF extraction. The HMF concentration was then quantified using spectrophotometry. Citrate@Fe3O4 exhibited a high surface area and strong interaction with HMF. We analyzed the individual influential factors affecting the magnetic solid phase extraction (MSPE) setup. Validation parameters were also provided to confirm the reliability of the method. Under optimal parameters, the method exhibited excellent linearity in the range of 0.05-30.00 µg/ml with the lower limit of quantification (LLOQ) of 0.05 µg/ml. Relative standard deviations (RSD) values for precision were better than 10% and the method's trueness were better than 10%. Recoveries were found to be in the range of 85% to 106%, indicating excellent accuracy and reliability. We used this method to identify and measure HMF in six different dextrose pharmaceutical dosage forms as intravenous injectable solutions and three honey samples.

Simultaneous derivatization and extraction of amphetamine and methamphetamine using dispersive liquid-liquid microextraction prior to their analysis using GC-FID in creatine supplements.

This study was focused on the development of a sensitive, reliable, and efficient extraction procedure for the determination of amphetamine and methamphetamine utilized in the adulteration of creatine sports supplements. The separation and detection of the analytes were conducted using the gas chromatography-flame ionization detection method. In this study, the analytes were extracted from a supplement powder into a proper solvent by sonication. Then, the extract was mixed with butyl chloroformate to obtain their butylated derivatives and then concentrated by a dispersive liquid-liquid microextraction procedure. The method was performed in a short time. Under optimized extraction conditions, a linear range of 2.01-500 ng g-1 was obtained by a coefficient of determination ≥0.996. Low detection (0.22 ng g-1 and 0.61 ng g-1 for amphetamine and methamphetamine, respectively) and quantification (0.73 ng g-1 and 2.01 ng g-1 for amphetamine and methamphetamine, respectively) limits, good precision (relative standard deviations ≤8.2%), and high extraction recoveries (79% and 86% for amphetamine and methamphetamine, respectively) were achieved. The usefulness of the method in the analysis of the target compounds was confirmed by studying the matrix effect and analysis of the analytes in different real samples.

Surfactant-enhanced air-agitation liquid-liquid microextraction of polycyclic aromatic hydrocarbons from edible oil using magnetic deep eutectic solvent prior to HPLC determination.

Herein, an air-agitation liquid-liquid microextraction procedure was developed for the extraction of several polycyclic aromatic hydrocarbons from edible oil samples. In this study, the extraction procedure was achieved using a new magnetic deep eutectic solvent as the extraction solvent, in which there was no need for centrifugation. To enhance the rate of extraction of the analytes from the samples, the method was promoted by the use of surfactant addition. The extracted analytes were determined by high-performance liquid chromatography with a diode array detector. The influence of various parameters on the extraction efficiency was studied by response surface methodology using a central composite design. Under optimal conditions, linear calibration curves for the target analytes were achieved in the range of 0.43-250 ng g-1. The limits of detection and quantification were in the ranges of 0.04-0.13 and 0.13-0.43 ng g-1, respectively. The repeatability of the method in terms of intra- and inter-day precision was ≤4.7% and ≤6.7%, respectively. The extraction recovery of the method ranged from 75 to 88%. The obtained results show that the proposed method is efficient for the analysis of the target analytes in various oil samples without obvious matrix effects. Pyrene was found in olive oil at a concentration of 42 ng g-1.

Development of homogeneous dispersive solid phase extraction using albumin as a green sorbent and its combination with dispersive liquid-liquid microextraction: application in extraction of pesticides from fruit juices.

In the current study, salt- and pH-induced homogeneous dispersive solid phase extraction was developed using albumin as a sorbent for the extraction of some pesticides (diazinon, diniconazole, haloxyfop-R-methyl, and hexaconazole) from fruit juice of orange, pomegranate, and barberry. The extracted analytes were more concentrated by dispersive liquid-liquid microextraction to obtain high enrichment factors and low detection limits prior to their determination by gas chromatography-mass spectrometry. In the extraction process, human serum albumin solution was added to the sample solution at the µL-level and a homogeneous solution was obtained. Then, albumin was precipitated into the solution by adding an inorganic salt and decreasing the solution pH. By doing so, the analytes were adsorbed by albumin effectively due to their high adsorption capacity and large surface area. Following this, the pesticides were eluted from the albumin sorbent using an elution solvent and used in a dispersive liquid-liquid microextraction step. Under the optimum extraction conditions, low limits of detection and quantification were achieved in the ranges of 0.02-0.04 and 0.07-0.13 ng mL-1, respectively. The calibration curves were linear in the range of 0.13-250 ng mL-1. Relative standard deviation as a criterion for precision and the method repeatability were in the ranges of 2.9-4.2% for intra- (n = 5, C = 5 or 50 ng mL-1) and 3.2-5.2% for inter-day (n = 5, 50 ng mL-1) precisions. The enrichment factors and extraction recoveries were in the ranges of 390-460 and 78-92%, respectively. Finally, the offered procedure was applied for the analysis of pesticide residues in some fruit juice samples.

Determination of metronidazole and clarithromycin in plasma samples using surfactant-modified amorphous carbon-based DSPE combined with DLLME followed by HPLC.

This work offers preparation of surfactant-modified amorphous carbon and its application in dispersive solid phase extraction of metronidazole and clarithromycin from plasma samples. The extraction procedure was combined with dispersive liquid-liquid microextraction for further preconcentration of the analytes for sensitive determination of the analytes followed by high performance liquid chromatography-diode array detector. In this work, first, the sorbent was added to the sample and the mixture vortexed to adsorb the analytes. Then, the obtained supernatant after centrifuging is discarded and the loaded analytes onto the sorbent surface were eluted with a water-miscible organic solvent. In the following, to further enrichment of the analytes the microextraction step was done. For this purpose, the eluate is taken, mixed with a water-immiscible organic solvent, and injected into deionized water. After centrifuging, an aliquat of the sedimented phase is taken and injected into the analytical instrument for the quantitative analysis. Under the optimum extraction conditions, high extraction recoveries (79 and 89% for metronidazole and clarithromycin, respectively), low limits of detection (2.1 and 1.9 ng mL-1 for metronidazole and clarithromycin, respectively) and quantification (7.0 and 6.3 ng mL-1 for metronidazole and clarithromycin, respectively), good repeatability (relative standard deviations less than 4.3% for intra- and 6.3% inter-day precisions), and wide linear ranges (7.3-1000 and 6.3-1000 ng mL-1 for metronidazole and clarithromycin, respectively) were obtained. At the end, the introduced method was applied on the plasma samples of the patients treated with metronidazole and clarithromycin successfully.

Liquid Phase Microextraction of Hazardous Compounds in Dairy Products; Principal and Practical Aspects.

Liquid phase microextraction techniques are considered as the miniaturized version of traditional liquid-liquid extraction, which use only several microliters of a proper solvent to extract the analytes from sample. In these methods, the target analytes are migrated into a water-immiscible organic solvent (acceptor phase) from an aqueous sample (donor phase). They are mainly classified into three main groups including (a) single-drop microextraction, (b) dispersive liquid-liquid microextraction, and (c) hollow fiber-liquid phase microextraction. These techniques have been successfully applied to the assessment of different analytes in food samples, pharmaceuticals, beverages, and so on. This review mainly focuses on up-to-date information on the application of liquid phase microextraction techniques in dairy products. The advantages and disadvantages of the developed liquid phase microextraction methods were discussed.

CuBTC metal organic framework-based dispersive solid phase extraction of cyclosporine and tacrolimus from plasma samples prior to determination by high performance liquid chromatography-tandem mass spectrometry.

Immunosuppressive drugs are prescribed to reduce the immune system of persons who are undergoing organ transplants. The concentration of these drugs in blood and plasma samples must be accurately and precisely determined during immunosuppressive therapy due to their significant side effects. In this study, a metal organic framework-based dispersive solid phase extraction method was developed for the extraction of tacrolimus and cyclosporine from plasma samples before their determination by high performance liquid chromatography-tandem mass spectrometry. For this purpose, CuBTC metal organic framework nanoparticles were prepared by a hydrothermal approach and they were used as the sorbent in the extraction procedure. The adsorbed analytes were eluted by a suitable organic solvent and then more concentrated by evaporation of the eluate. All of the effective parameters of the method including sorbent amount, adsorption time, eluent type, desorption time, eluent volume, and sample solution pH were studied and optimized. They were obtained 5 mg, 5 min, acetone, 5 min, 300 µL, and 5, respectively. Under optimal conditions, the developed method was validated and the data showed that the linear range, the limit of detection, the limit of quantification, the coefficient of determination, the enrichment factor, and relative standard deviation values were 1-1000 ng mL-1, 0.30 ng mL-1, 0.5 ng mL-1, 0.99, 15.6, and 5.8 % for tacrolimus and 0.8-500 ng mL-1, 0.25 ng mL-1, 0.4 ng mL-1, 0.99, 17, and 5.6 % for cyclosporine, respectively. Finally, the method was successfully used in the determination of the studied drugs in plasma samples.

Dispersive solid phase extraction of metronidazole and clarithromycin from human plasma using a ß-cyclodextrin grafted polyethylene polymer composite.

In this work, for the first time, a polymeric composite based on ß-cyclodextrin grafted with polyethylene has been prepared through ball milling and used as an efficient sorbent for dispersive solid phase extraction of metronidazole and clarithromycin from plasma samples. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffraction, and scanning electron microscopy. In the extraction process, after precipitating the proteins, the sorbent was added into the sample solution, and the mixture was vortexed to facilitate and speed up the sorption of the analytes onto the sorbent surface. After centrifuging, the sorbent particles were contacted with methanol to elute the analytes under the vortexing process. After this step, an aliquot of the eluate was taken and injected into high-performance liquid chromatography-diode array detector for quantitative analysis. Under the optimum extraction conditions, the extraction recoveries for metronidazole and clarithromycin were 76 and 83%, respectively. The limits of detection were 2.6 and 2.2 ng/ml for metronidazole and clarithromycin, respectively. The repeatability of the offered approach, expressed as relative standard deviation, was equal to or less than 4.7%. Finally, the method was successfully applied to plasma samples of the patients treated with metronidazole and clarithromycin.

Recent Advances in Impedimetric Biosensors Focusing on Myocardial Infarction Diagnosis.

Acute myocardial infarction is the most common cardiovascular disease and 85% of cardiovascular disease-related deaths are associated with it. The variation in the cardiac troponin concentration is considered as the most significant judge index for acute myocardial infarction diagnosis. Here, a comprehensive insights is given about the impedimetric methods as powerful electrochemical biosensing platforms for cardiac troponin evaluation. Focusing on nano materials, various impedimetric techniques including faradaic and non-faradaic techniques and different transducer modification techniques are addressed. The steps taken by each of the studied platforms to solve the existing problems are discussed and their advantages and drawbacks are highlighted. A glance at the provided table is given a mind into the features of each impedimetric sensors and their comparison are provided.

UiO-66-based metal-organic framework for dispersive solid-phase extraction of vanillylmandelic acid from urine before analysis by capillary electrophoresis.

Dispersive solid-phase extraction (DSPE) was developed for the extraction of vanillylmandelic acid (VMA) in urine samples prior to capillary electrophoresis with diode array detection (CE-DAD). Extraction of VMA by DSPE was carried out by direct addition of 7.5 mg of synthesized amino-functionalized UiO-66 (Zr) metal-organic framework adsorbent into the 5 mL sample solution (pH 4.0), followed by sonication and centrifugation. The supernatant layer was discarded, then the sedimented adsorbent was eluted using borate buffer (75 mM, pH 10). Effective extraction parameters including the amount of adsorbent, sample pH, adsorption and desorption time, type, volume and pH of eluent, and type of adsorbent dispersion method were systematically investigated. Under the optimized conditions, linearity of the method was from 40 to 2000 µg L-1 with a correlation coefficient over 0.9948. The method detection and quantification limits were 12 and 40 µg L-1, respectively. The relative standard deviations for intra-and inter-day precision were 2.4 and 2.8% (n = 5), respectively. The extraction recovery and enrichment factor values were 90% and 9.0 respectively.

A modified quick-easy-cheap-effective-rugged-and-safe method involving carbon nano-onions-based dispersive solid-phase extraction and dispersive liquid-liquid microextraction for pesticides from grapes.

A combination of modified quick easy cheap effective rugged and safe extraction approach with carbon nano-onions-based dispersive solid-phase extraction and dispersive liquid-liquid microextraction was developed for the extraction of several pesticides (diazinon, chlorpyrifos, tebuconazole, deltamethrin, permethrin, haloxyfop-methyl, penconazole, and cyhalothrin) from grape before their analysis by gas chromatography-flame ionization detection. In the extraction approach, an aliquot of grape sample is chopped and after separating its juice, the pesticides that remained in the refuse are extracted by the quick, easy, cheap, effective, rugged, and safe extraction method. The obtained acetonitrile phase is mixed with juice and the analytes are extracted by the carbon nano-onions-based dispersive solid-phase extraction. The analytes are concentrated using the microextraction procedure to obtain high enrichment factors. The results showed low limits of detection (0.5-1.6 ng/g) and quantification (1.8-5.4 ng/g) with satisfactory linearity of the calibration curves (determination coefficient, r2 ≥ 0.994). The precision of the developed method expressed as relative standard deviations was good (≤7.2%). The method provided high enrichment factors (350-410) and extraction recoveries (70-82%). Finally, seven grape samples were analyzed successfully.

A mixed deep eutectic solvents-based air-assisted liquid-liquid microextraction of surfactants from exhaled breath condensate samples prior to HPLC-MS/MS analysis.

A ternary solvent system-based air-assisted liquid-liquid microextraction procedure was developed for the extraction of three surfactants from exhaled breath condensate samples prior to their determination by high performance liquid chromatography-tandem mass spectrometry. In this approach, different deep eutectic solvents were synthesized based on phosphocholine chloride and fatty acids and their mixtures were used as the extraction solvents to effective extraction of the analytes. To obtain the optimum composition of the extraction solvents, a simplex centroid design approach was used. Then the effective parameters were studied by response surface methodology using central composite design. The obtained data after optimization showed that 6 times was the best extraction time for the developed procedure. When the sample solution pH was adjusted at 3.7, the method reached to higher extraction efficiency which can be related to the fact that the analytes were in the protonated forms. Increasing the sample solution temperature up to 50 °C enhanced the migration rate of the analytes into the extraction solvent and the method efficacy was increased. Also addition of sodium chloride at 2.8% (w/v) had a positive effect on the method efficiency which can be related to decreasing the analytes solubility in the sample solution. Under optimal conditions, the method showed satisfactory coefficient of determination (≥0.9979), low limit of detection (0.12-0.23 ng mL-1) and quantification (0.39-0.76 ng mL-1), acceptable repeatability in deionized water (relative standard deviation ≤ 8.2%) and in exhaled breath condensate (relative standard deviation ≤ 7.2%), and acceptable extraction recovery (75-86%) and enrichment factor (71-86). Considering these results, the developed method provided a quick and efficient way to determine surfactants in the exhaled breath condensate collected from expiratory circuit of the mechanical ventilator. It can be used in drug monitoring and clinical studies.

In-situ sorbent formation for the extraction of pesticides from honey.

An organic polymer was re-precipitated in solution to use as an adsorbent in dispersive solid-phase extraction of some pesticides from honey samples prior to their determination by high-performance liquid chromatography-tandem mass spectrometry. In this approach, different deep eutectic solvents were prepared using lysine and their ability in elution of the analytes from the adsorbent surface was tested. A diluted honey solution was transferred into a glass test tube and then a solution of polystyrene dissolved in dimethylformamide was injected into the solution. By doing this, polystyrene is re-precipitated in the solution and dispersed in whole parts of it as many tiny particles. Then the mixture was centrifuged and the adsorbed analytes on the particles were eluted using a proper hydrophilic deep eutectic solvent. The central composite design approach was used for the optimization of effective parameters. The limits of detection and quantification were in the ranges of 0.06-0.20 and 0.22-0.69 ng/g, respectively. The calibration curves obtained by matrix-matched standard solutions were linear in the range of 0.69-500 ng/g with a coefficient of determinations ≥0.9962. The method provided high extraction recoveries (70-99%) and enrichment factors (140-198), and an acceptable precision (relative standard deviations ≤7.1%).

Dispersive micro-solid-phase extraction of aflatoxins from commercial soy milk samples using a green vitamin-based metal-organic framework as an efficient sorbent followed by high performance liquid chromatography-tandem mass spectrometry determination.

In the current work, for the first time, a vitamin-based metal-organic framework constructed from cobalt ions and vitamin B3 has been used as a sorbent in dispersive micro-solid-phase extraction. The proposed method was used to extract and enrich aflatoxins (B1, B2, G1, and G2) from soy milk samples before their quantification by high performance liquid chromatography-tandem mass spectrometry. In this work, first the metal-organic framework was synthesized and characterized using techniques such as X-ray diffraction, Fourier transform infrared spectrophotometry, scanning electron microscopy, nitrogen adsorption/desorption, and energy-dispersive X-ray spectroscopy. Then it was used as an efficient sorbent in the proposed dispersive micro-solid-phase extraction. For this purpose, after precipitating the proteins of soy milk sample with the aid of trichloroacetic acid, the supernatant phase was taken, mixed with the synthesized sorbent, and vortexed. After centrifuging, the analytes loaded on the adsorbent were eluted with methanol to transfer them into an organic phase which was compatible with the subsequently employed separation system. The adsorption capacity of the synthesized MOF for aflatoxins B1, B2, G1, and G2 were 0.77, 0.83, 0.70, and 0.54 mg g-1, respectively. Under the best experimental situations, satisfactory outcomes including acceptable extraction recoveries (64-75%), low limits of detection (11.3-48.2 ng L-1) and quantification (42.8-161.6 ng L-1), and good repeatability (relative standard deviations equal or less than 4.0 and 4.7% for intra- and inter- day precisions, respectively) were obtained. In addition, green synthesis of the metal-organic framework (using vitamin B3 as a linker, water as the reaction solvent, and mild conditions) and usage low amount or volume of the adsorbent and organic solvents during the extraction process were the other beneficial aspects of this work which caused the suggested analytical method to be environmentally friendly.

Evaluation of MXene as an adsorbent in dispersive solid phase extraction of several pesticides from fresh fruit juices prior to their determination by HPLC-MS/MS.

This study aimed to introduce a dispersive solid phase extraction method based on MXene nanoparticles as a novel sorbent for the simultaneous extraction and determination of twelve pesticides from fresh fruit juices. In the following, a high performance liquid chromatography-tandem mass spectrometry was used for their determination in the samples. In this method, two-dimensional nanomaterials of Ti2AlC were exfoliated in an acidic solution and then they were added into the sample solution. To enhance the sample solution and sorbent contact area, the mixture was vortexed for a few minutes. Then the adsorbed analytes onto the sorbent were eluted using acetone and then analyzed. Under optimal conditions, the calibration curves of the method were linear within the range of 3.0-1000 µg L-1. The limits of detection, intra- and inter-day relative standard deviations, and extraction recoveries were in the ranges of 0.08-1.0 µg L-1, 2.5-4.2%, 2.5-5.5%, and 69-75%, respectively. Performing the method verified the presence of some of the analytes in several samples. This method can help to monitor pesticides in juice samples as well as to improve our understanding the safety of foods.

Application of calcium oxide as an efficient phase separation agent in temperature-induced counter-current homogenous liquid-liquid extraction of aflatoxins from dried fruit chips followed by high-performance liquid chromatography-tandem mass spectrometry determination.

A temperature-induced counter-current homogenous liquid-liquid extraction procedure performed in a burette has been proposed for the isolation of aflatoxins B1, B2, G1, and G2 from various fruit chip samples. In this method, a homogenous solution of deionized water and cyclohexylamine is added to the solid sample and the resulted mixture is vortexed. In the following, the liquid phase is taken and passed through the burette filled with a mixture of calcium oxide (as a phase separation agent) and sand (to avoid clumping the calcium oxide). By doing so, the temperature of the solution is increased by hydration of calcium oxide and consequently, the homogenous state is broken and the aflatoxins are migrated into the resulted tiny droplets of cyclohexylamine. This phase is collected on the top of the solution owing to its low density with respect to an aqueous solution. Numerous parameters which can affect the efficiency of the suggested approach were evaluated and under the best situations, great repeatability, low limits of determination and quantification, and high extraction recoveries were acquired. In the end, the suggested approach was employed for the quantification of the selected aflatoxins in various fruit chips samples marketed in Tabriz City, Iran.