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    Reza Mogaddam

    In this study, a new floating dispersive solid phase extraction method based on deep eutectic solvents has been developed in a home-made extraction device for the extraction of four tetracycline antibiotics from milk samples. In this... more
    In this study, a new floating dispersive solid phase extraction method based on deep eutectic solvents has been developed in a home-made extraction device for the extraction of four tetracycline antibiotics from milk samples. In this approach, the sorbent (activated carbon) was dispersed in whole parts of solution with the aid of air stream and floated on top of the solution with the aid of the surfactant (lauryl betaine) and air bubbles. After collection of the sorbent, the adsorbed analytes were eluted with tetrabutyl ammonium chloride-propionic acid deep eutectic solvent under sonication. In this method, there was no need to organic dispersive and extraction solvents and the used sorbent was collected on top of the solution and collected without centrifugation. The validation parameters showed that low limits of detection (0.1-0.3 μg kg-1 ) and quantification (0.6-1.0 μg kg-1 ), acceptable enrichment factors (52-60), efficient extraction recoveries (80-91%), and satisfactory relative standard deviations (≤9.8%) were obtained. Eventually, the method was successfully applied on different milk samples and tetracycline was determined in them. This article is protected by copyright. All rights reserved.
    Background: Because of the narrow therapeutic range of tricyclic antidepressant drugs, their determination in biological samples is of great importance. In this work, a fast and environment friendly sample pretreatment method based on a... more
    Background: Because of the narrow therapeutic range of tricyclic antidepressant drugs, their determination in biological samples is of great importance. In this work, a fast and environment friendly sample pretreatment method based on a dispersive liquid–liquid microextraction was developed for the extraction and preconcentration of four tricyclic antidepressants including nortriptyline, amitriptyline, desipramine, and clomipramine in urine prior to their determinations by gas chromatography–mass spectrometry. Methods: In the suggested method, an appropriate mixture of Na2SO4 solution (as phase separation agent and disperser) containing iso–propanol (extraction solvent) is rapidly injected into an alkaline aqueous sample solution containing Na2SO4 and the analytes. As a result, a cloudy mixture is formed and the tiny droplets of the extractant containing the extracted analytes are collected on the surface of the aqueous phase after centrifuging. Finally, an aliquot of the collected ...
    A new approach to continuous homogeneous liquid–liquid microextraction based on the solidification of organic droplets has been developed in a newly designed home-made extraction device for the extraction and preconcentration of... more
    A new approach to continuous homogeneous liquid–liquid microextraction based on the solidification of organic droplets has been developed in a newly designed home-made extraction device for the extraction and preconcentration of organothiophosphate pesticides from different fruit juices and vegetable samples prior to gas chromatography-mass spectrometry. In the present work, two parallel glass tubes with different lengths and diameters were connected together with a stopcock in which cool water was circulated from the wide side of them. This was used as the extraction device. Firstly, a homogeneous phase containing the sample solution and an extraction solvent (cyclohexanol) was filled into the wide diameter side of the device. Then sodium sulfate solution placed into the other side of the device was flowed into the homogeneous solution to release the extraction solvent from the solution. Along with the flowing of sodium sulfate, cool water was circulated from the wide side of the d...
    A new liquid-liquid microextraction approach by applying a deep eutectic solvent was adopted for the extraction of four antibiotics (penicillin G, dihydrostreptomycin, enrofloxacin, and ciprofloxacin) from honey samples. The enriched... more
    A new liquid-liquid microextraction approach by applying a deep eutectic solvent was adopted for the extraction of four antibiotics (penicillin G, dihydrostreptomycin, enrofloxacin, and ciprofloxacin) from honey samples. The enriched analytes were analyzed by HPLC-MS/MS. The procedure was carried out by synthesis of tetrabutylammonium chloride: p-cresol deep eutectic solvent in the sample solution and then its decomposition in the presence of an acid. In-solution formation of deep eutectic solvent provided wide contact areas among the extractant and sample solution, and accelerated sample preparation. Also, its decomposition enabled collection of the final extraction phase without centrifugation. Low LODs (0.55-0.79 ng/g) and LOQs (1.9-2.6 ng/g), high ERs (70-92%), and suitable RSDs (≤ 6.9%) were obtained. After performing the method on real samples, dihydrostreptomycin was found in several honey samples.
    In this work, a simple, inexpensive, green, and fast dispersive micro-solid phase extraction method has been developed for the extraction of several pesticides from honey samples.
    A new amorphous carbon-based dispersive micro solid-phase extraction method was developed for the extraction and preconcentration of several mycotoxins from soymilk samples.
    In this paper, a fast, sensitive, and selective sample preparation procedure was presented for the determination of 3-monochloropropane-1,2-diol (3-MCPD) in refined edible oils using gas chromatography-mass spectrometry. In this method,... more
    In this paper, a fast, sensitive, and selective sample preparation procedure was presented for the determination of 3-monochloropropane-1,2-diol (3-MCPD) in refined edible oils using gas chromatography-mass spectrometry. In this method, firstly, the sample lipids and analyte fatty esters are saponified by sodium hydroxide under sonication. After that the analyte was derivatized using phenylboronic acid (as the derivatization agent) and the obtained derivative was extracted during an air-assisted liquid-liquid microextraction procedure (AALLME). Six different deep eutectic solvents (DESs) were prepared as the extraction solvents and the most effective extraction for 3-MCPD was obtained in the presence of a natural DES (NDES) consisting of choline chloride (ChCl)-acetic acid (AcOH). Important variables such as sodium hydroxide concentration and volume, sonication time, temperature, extraction solvent type and volume, and phenylboronic acid concentration and volume have been optimized. Using the optimum conditions, broad linear range (0.88-1000 ng g-1), suitable coefficient of determination (0.995), and low limits of detection (0.26 ng g-1) and quantification (0.88 ng g-1) were obtained. Relative standard deviations for intra- (n=8) and inter-day (n=6) precisions at a concentration of 5 ng g-1 were 2.6 and 3.2%, respectively. The developed method has been successfully applied to 3-MCPD determination in refined edible oil samples including sunflower, corn, and canola oils.
    A green, simple, and efficient dispersive micro solid phase extraction method was developed for the extraction of polycyclic aromatic hydrocarbons from honey samples. In this method, for the first time, curcumin was used as an efficient... more
    A green, simple, and efficient dispersive micro solid phase extraction method was developed for the extraction of polycyclic aromatic hydrocarbons from honey samples. In this method, for the first time, curcumin was used as an efficient and green sorbent to extract the analytes from the sample. After that, the adsorbed analytes were eluted using a deep eutectic solvent prepared by mixing tetrabutylammonium chloride: ethylene glycol and analyzed by gas chromatography-mass spectrometry. Important experimental factors affecting adsorption and desorption steps of the method were optimized and under optimal experimental conditions, low limits of detection (0.14-0.37 ng g-1 ) and quantification (0.49-1.3 ng g-1 ), wide linear range (1.3-500 ng g-1 ) with a coefficient of determination ≥0.994 were obtained. Relative standard deviation values for intra- and inter-day precisions were ≤7.5% for all of the analytes at a concentration of 2 ng g-1 for each analyte (n = 6). Extraction recovery of the method was in the range of 72-81%. Finally, twenty honey samples were analyzed and the analytes were successfully detected. The method is environment friendly because of the use of curcumin as a sorbent. Also, biodegradability of the used deep eutectic solvent components is another advantage of the method. This article is protected by copyright. All rights reserved.
    Polystyrene-polyricinoleic acid copolymer containing silver nano particles (AgPSrici) was synthesized and used in separation of molybdenum from different aqueous and foodstuff samples during a dispersive-µ-solid phase extraction approach.... more
    Polystyrene-polyricinoleic acid copolymer containing silver nano particles (AgPSrici) was synthesized and used in separation of molybdenum from different aqueous and foodstuff samples during a dispersive-µ-solid phase extraction approach. The synthesized nano particles were verified using Fourier transform infraredspectroscopy. An electrothermal atomic absorption spectrometry has been used for measurement of the studied ions. AgPSrici amount pH, sample volume, elution solvent kind, and the time of extraction were the effective parameters that were optimized by one-variable-at-one-time method. Analytical data of the method was calculated and limit of detection, relative standard deviation, limit of quantification were 0.022 µg L-1, 2.9%, 150, and 0.066 µg L-1, respectively. The synthesized adsorption capacity was obtained 170 mg g-1.Accuracy of the method was studied by performing the method on certified reference materials and the presence of different interfering ions was studied. Molybdenum content of different water and foodstuffs was determined by the introduced method.
    A cold-induced-homogeneous liquid–liquid extraction method combined with deep eutectic solvent-based dispersive liquid–liquid microextraction has been done to extract several endocrine disrupting compounds (phenol, p-chlorophenol,... more
    A cold-induced-homogeneous liquid–liquid extraction method combined with deep eutectic solvent-based dispersive liquid–liquid microextraction has been done to extract several endocrine disrupting compounds (phenol, p-chlorophenol, p-nitrophenol, octylphenol, methyl paraben, ethyl paraben, butyl paraben, and bisphenol A) and hydroxymethylfurfural from honey samples before their determination by gas chromatography–mass spectrometry. In this method, two ternary deep eutectic solvents including tetrabutyl ammonium chloride: dichloroacetic acid: ethylene glycol (hydrophilic) and tetrabutyl ammonium chloride: dichloroacetic acid: decanoic (hydrophobic) acid deep eutectic solvents are prepared and used as the extraction solvents in the developed method. The analytes are extracted by a two-step extraction procedure in which they are first extracted into the hydrophilic deep eutectic solvent and then transferred into a few microliters of the hydrophobic deep eutectic solvent for more concentration. In both steps, phase separation is done by centrifugation at low temperature. The method was optimized and validated and the results showed that the method had low limits of detection (0.21–0.50 ng g−1) and quantification (0.72–1.7 ng g−1), wide liner ranges, and an acceptable repeatability (relative standard deviation≤12). Lastly, the developed method was applied on different honey samples and bisphenol A, p-nitrophenol, and hydroxymethfurfural were found in some of them.
    In this research, MIL-68 (Al) was synthesized and used for the extraction of some plasticizers from various samples stored in plastic bottles.
    An efficient, rapid, simple and repeatable sample preparation method based on pressurised liquid extraction combined with deep eutectic solvent-based dispersive liquid–liquid microextraction was de...
    In the present work, a new and efficient sample treatment method based on the combination of stirring-dependent magnetic dispersive solid phase microextraction and ferrofluid-based dispersive liquid–liquid microextraction has been... more
    In the present work, a new and efficient sample treatment method based on the combination of stirring-dependent magnetic dispersive solid phase microextraction and ferrofluid-based dispersive liquid–liquid microextraction has been developed for the extraction of some pyrethroid pesticides (bifenthrin, phenothrin, tetramethrin, cyhalothrin, permethrin, and cypermethrin) from fruit juices prior to their determination with gas chromatography–mass spectrometry. For this purpose, a few milligrams of a synthesized magnetic sorbent (Fe3O4@polythiophene) is added into a sample solution containing the analytes and stirred at high rate. By this action, particles of the magnetic sorbent are detached from the magnetic stir bar surface and completely dispersed throughout the solution. After stopping stirring, the particles containing the adsorbed analytes are rapidly returned onto the stir bar. Then, the stir bar is taken and eluted with an appropriate solvent to desorb the analytes. Afterward, the eluent is mixed with a few microliters of a synthesized ferrofluid and the mixture is rapidly injected into deionized water placed in a conical glass test tube for more enrichment of the analytes. In the next step, the ferrofluid settled down at the bottom of the tube in the presence of an external magnet and the supernatant is discarded. After back-extraction of the analytes with n-hexane, an aliquot of the extract is injected into the determination system. Under optimal conditions, the developed method offered high enrichment factors (1380–1660) and extraction recoveries (69–83%), and low limits of detection (4.0–12 ng L−1) and quantification (14–40 ng L−1). The relative standard deviations were ≤ 7.1% for intra-day (n = 6) and inter-day (n = 4) precisions at a concentration of 250 ng L−1 of each analyte. Finally, six different fruit juice samples were successfully analyzed by the introduced method and cypermethrin was detected in apple juice at a concentration of 110 ± 0.5 ng L−1.
    In present work, a sample pre-treatment method based on a combination of homogenous liquid–liquid extraction and dispersive liquid–liquid microextraction has been proposed for the extraction of som...
    In-situ synthesis of a deep eutectic solvent and homogenous liquid-liquid microextraction performed in a narrow bore tube was developed for efficient extraction of irgaphos 168 and irganox 1010 in doogh and water samples packed in... more
    In-situ synthesis of a deep eutectic solvent and homogenous liquid-liquid microextraction performed in a narrow bore tube was developed for efficient extraction of irgaphos 168 and irganox 1010 in doogh and water samples packed in polypropylene packages. Firstly pH of the aqueous sample solutions containing the analytes is adjusted at 9. Then a hydrogen bond acceptor (choline chloride) and a hydrogen bond donor (oleic acid) are dissolved in the solution and vortexed to obtain a homogenous solution. The solution is filled into a narrow bore tube which its bottom was clogged by a septum. Then hydrochloric acid solution is injected into the solution by a syringe. The tube is placed in an ultrasonic. During this step the droplets of choline chloride: oleic acid deep eutectic solvent are produced. The method indicated high enrichment factor (435 for irgaphos 168 and 488 for irganox 1010), low limits of detection (0.03 and 0.09 ng mL-1 for irgaphos 168 and irganox 1010, respectively) and quantification (0.13 and 0.29 ng mL-1 for irgaphos 168 and irganox 1010), good recovery (74 and 83% for Irgaphos 168 and Irganox 1010, respectively), and satisfactory repeatabilities (relative standard deviations≤ 12%) can be obtained using the develop method. This article is protected by copyright. All rights reserved.
    Abstract In the present study a liquid phase microextraction method has been developed using new kind of solvents named deep eutectic solvents, for the extraction and preconcentration of some pesticides from different samples including... more
    Abstract In the present study a liquid phase microextraction method has been developed using new kind of solvents named deep eutectic solvents, for the extraction and preconcentration of some pesticides from different samples including apple, grape and sour cherry juices and fresh beet, cucumber, potato, and tomato. In this work, a deep eutectic solvent has been synthesized using a hydrogen bonding donor (p–chlorophenol) and hydrogen bonding acceptor (choline chloride), then used as an extraction solvent. Dispersion of the extraction solvent into the aqueous phase was performed by temperature changing. Dispersion of deep eutectic solvent had dramatically enhanced by the developed method which led to the improvement of extraction efficiency of the method. Under the optimum extraction conditions, enrichment factors and extraction recoveries were obtained in the ranges of 280–465 and 56–93%, respectively. Low limits of detection and quantification were obtained in the ranges of 0.13–0.31 and 0.45–1.1 ng mL−1, respectively. Relative standard deviations were less than 9%, for the extraction of 50 ng mL−1of each pesticide which obtained for intra- (n = 6) and inter-day (n = 4) precisions. Application of the method on the studied samples were free of the analytes, except tomato in which diazinon was detected at a concentration of 62 ng g−1.
    Please cite this article in press as: M.A. Farajzadeh, et al., Corrigendum to “Development of a new microextraction method based on elevated temperature dispersive liquid–liquid microextraction for determination of triazole pesticides... more
    Please cite this article in press as: M.A. Farajzadeh, et al., Corrigendum to “Development of a new microextraction method based on elevated temperature dispersive liquid–liquid microextraction for determination of triazole pesticides residues in honey by gas chromatography-nitrogen phosphorus detection” [J. Chromatogr. A 1347 (2014) 8-16], J. Chromatogr. A (2017), https://doi.org/10.1016/j.chroma.2017.11.040 The authors regret that the order of authors “Mir Ali Farajzadeh, Mohammad Reza Afshar Mogaddam, Houshang Ghorbanpour” must e corrected to “Mohammad Reza Afshar Mogaddam, Mir Ali Farajzadeh, Houshang Ghorbanpour”. The authors would like to apologise for any inconvenience caused.
    In the present work, a simultaneous derivatization and air-assisted liquid-liquid microextraction method based on the solidification of deep eutectic solvent coupled with gas chromatography-mass spectrometry has been developed for the... more
    In the present work, a simultaneous derivatization and air-assisted liquid-liquid microextraction method based on the solidification of deep eutectic solvent coupled with gas chromatography-mass spectrometry has been developed for the determination of some aromatic amines in various aqueous samples. In this work, choline chloride and n-butyric acid are mixed at a suitable molar ratio and after heating, a deep eutectic solvent of low density compared to water is formed. The prepared extraction solvent is mixed with ethyl chloroformate as a derivatization agent and injected into an alkaline aqueous solution containing the target analytes adjusted at elevated temperature. The resulting mixture is drawn into a syringe via a needle and pushed out into a test tube several times. As a result, a cloudy solution consisting of the fine droplets of the extraction solvent containing the derivatized aromatic amines is obtained. Then, the solution is placed into an ice bath and the extraction solvent is solidified and collects on the top of the solution after centrifugation. Then the solidified extraction solvent is removed by a spatula and transferred to a microtube and dissolved in 10 μL acetonitrile. A portion of the obtained mixture is injected into the gas chromatography-mass spectrometry. Under optimum conditions, limits of detection and quantification were obtained in the ranges of 1.8-6.0, and 6.0-23 ng L-1, respectively. The extraction recoveries, enhancement factors, and enrichment factors of the selected aromatic amines ranged from 79-94%, 2498-3422 and 790-940, respectively. The relative standard deviations were ≤5.3% for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 100 ng L-1 of each analyte.
    Simultaneous derivatization and air-assisted liquid-liquid microextraction using an organic solvent lighter than water has been developed for the extraction of some parabens in different samples with the aid of a newly designed device for... more
    Simultaneous derivatization and air-assisted liquid-liquid microextraction using an organic solvent lighter than water has been developed for the extraction of some parabens in different samples with the aid of a newly designed device for collecting the extractant. For this purpose, the sample solution is transferred into a glass test tube and a few microliters of acetic anhydride (as a derivatization agent) and p-xylene (as an extraction solvent) are added to the solution. After performing the procedure, the homemade device consists of an inverse funnel with a capillary tube placed into the tube. In this step, the collected extraction solvent and a part of the aqueous solution are transferred into the device and the organic phase indwells in the capillary tube of the device. Under the optimal conditions, limits of detection and quantification for the analytes were obtained in the ranges of 0.90-2.7 and 3.0-6.1 ng mL , respectively. The enrichment and enhancement factors were in the...
    In the present study, a new, simple, rapid, and environmentally friendly headspace-liquid phase microextraction method followed by gas chromatography–flame ionization detection has been developed for the extraction/preconcentration and... more
    In the present study, a new, simple, rapid, and environmentally friendly headspace-liquid phase microextraction method followed by gas chromatography–flame ionization detection has been developed for the extraction/preconcentration and determination of 1,4-dioxane from shampoo. The developed procedure is performed in a home-made extraction vessel, connected to a glass vial containing sample and extraction solvent. In this method, an aliquot weight of shampoo is mixed with a binary mixture of n-hexane and dichloromethane (50:50, v/v) as the extractant and the target analyte is extracted during a liquid–liquid extraction procedure. Then a home-made extraction vessel containing a few microliters of a collection/extraction solvent is contacted to a glass vial containing the organic phase obtained from the previous step. By heating 1,4-dioxane is vaporized and enriched in a μL volume of the collection/extraction solvent. Then an aliquot volume of the collected phase is injected into the separation system. The effect of several factors which may influence performance of the method, including kind and volume of the extraction solvents used in both steps, extraction temperature, extraction time, and salt addition were evaluated. Under the optimum extraction conditions, limits of detection and quantification for the target analyte were obtained 0.52 and 1.73 μg kg−1, respectively. Enrichment factor and extraction recovery were 333 and 89 %, respectively. The method precision was evaluated at a concentration of 25 μg kg−1 and relative standard deviation was less than 6.9 % for intra-day (n = 6) and inter-day (n = 4) precisions. Finally, the proposed method has been successfully applied in analysis of 1,4-dioxane in different shampoo samples.
    New generation of solvents, named deep eutectic solvents, were simultaneously synthesized and used as an extraction solvent in a liquid–liquid microextraction method for the extraction and preconcentration of some polycyclic aromatic... more
    New generation of solvents, named deep eutectic solvents, were simultaneously synthesized and used as an extraction solvent in a liquid–liquid microextraction method for the extraction and preconcentration of some polycyclic aromatic hydrocarbons.
    In this paper, a new version of HLLE based on an acid–base reaction combined with DLLME followed by GC-FID has been developed for the extraction and determination of aryloxyphenoxy-propionate pesticides in fruit juice and vegetable samples.
    Sherry brandy (Jerez, SW, Spain) is a high quality distilled beverage derived from wine. Its perceived quality depends, inter alia, on hundreds of flavour compounds. A Stir Bar Sorptive Extraction (SBSE) method coupled to gas... more
    Sherry brandy (Jerez, SW, Spain) is a high quality distilled beverage derived from wine. Its perceived quality depends, inter alia, on hundreds of flavour compounds. A Stir Bar Sorptive Extraction (SBSE) method coupled to gas chromatography-mass spectrometry has been developed for the analysis of volatile compounds in Sherry brandy. The optimization of the extraction procedure has been carried out using a statistical approach, based on a factorial design. The best overall analytical conditions obtained were the following: 35 mL of sample, diluted 1:1 with Milli-Q water and extraction at 1100 rpm for 100 min. The method has been successfully validated in a further stage of this work. Several performance characteristics such as calibration, linearity, precision (inter- and intra-assay), detection and quantification limits and recovery were studied. Finally, the method developed has been applied to different Sherry brandies. The results obtained show SBSE to be a suitable technique for the reliable analysis of volatile compounds in brandies.
    A dispersive solid-phase microextraction method based on magnetic carbon nano-onions (MCNOs) was developed for the extraction and preconcentration of some pesticides from water and vegetable samples.
    An ultrasound-assisted homogenous liquid-liquid microextraction method using a new deep eutectic solvent was proposed for the extraction of daclatasvir and sofosbuvir from urine. The analytes were determined by high performance liquid... more
    An ultrasound-assisted homogenous liquid-liquid microextraction method using a new deep eutectic solvent was proposed for the extraction of daclatasvir and sofosbuvir from urine. The analytes were determined by high performance liquid chromatography-diode array detector. The deep eutectic solvent was prepared by mixing p-aminophenol with tetrabutyl ammonium chloride. It was used in the extraction procedure as an extraction solvent. The amine group in structure of the prepared deep eutectic solvent led to its various solubility in different pHs. In this method, urine sample was placed in a glass test tube and then mixed with sodium chloride and its temperature adjusted at 50 °C. Then, the deep eutectic solvent was dissolved in the solution by manually shaking. In the following, an ammonia solution was added to the solution and the mixture was sonicated for 4 min. After centrifugation, an aliquat of the sedimented phase was injected into the determination system. Low limits of detection (daclatasvir 1.0 and sofosbuvir 1.3 μg/L) and quantification (daclatasvir 3.3 and sofosbuvir 4.0 μg/L), high enrichment factor (daclatasvir 96 and sofosbuvir 90) and extraction recovery (daclatasvir 96 and sofosbuvir 90 %), and good percision (relative standard deviation ≤9.3 %) were obtained. The introduced method was successfully applied in the determination of daclatasvir and sofosbuvir concentrations in urine samples.
    A new extraction procedure based on combination of a solvent extraction and deep eutectic solvent-based dispersive liquid-liquid microextraction has been introduced for the extraction of aflatoxin M1 from cheese samples. In this method,... more
    A new extraction procedure based on combination of a solvent extraction and deep eutectic solvent-based dispersive liquid-liquid microextraction has been introduced for the extraction of aflatoxin M1 from cheese samples. In this method, acetonitrile, deionized water, and n-hexane are added onto the sample and vortexed. Owning to different affinities of the substances in cheese towards the mentioned solvents, an efficient and selective extraction of the analyte is done into the acetonitrile phase. After centrifugation, acetonitrile phase is removed and mixed with a new hydrophobic deep eutectic solvent prepared from N,N-diethanol ammonium chloride and carvacrol as an extraction solvent. The mixture is injected into deionized water and a cloudy solution is obtained. Eventually, an aliquot of the organic phase is injected into high performance liquid chromatography-fluorescence detection. After optimizing the effective parameters with the response surface methodology and a quadratic model, limits of detection and quantification were 0.74 and 2.56 ng kg-1 , respectively. The obtained extraction recovery and enrichment factor were 94% and 94, respectively. Also, intra- (n = 6) and inter-day (n = 4) precisions were less than or equal to 8.6% at a concentration of 5 ng kg-1 . The suggested method was applied to determine aflatoxin M1 in different cheese samples. This article is protected by copyright. All rights reserved.
    In this work, a microwave-enhanced air-assisted liquid-liquid microextraction method combined with gas chromatography-mass spectrometry has been developed for morphine and oxymorphone assessment in EBC samples. For this purpose, choline... more
    In this work, a microwave-enhanced air-assisted liquid-liquid microextraction method combined with gas chromatography-mass spectrometry has been developed for morphine and oxymorphone assessment in EBC samples. For this purpose, choline chloride-menthol-phenylacetic acid deep eutectic solvent (as an extraction solvent), butyl chloroformate (as a derivatization agent), and picoline (as a catalyst) are used. After performing predetermined extraction cycles in the microextraction method, the obtained cloudy solution is exposed to microwave irradiations to enhance extraction and derivatization efficiencies. The method provided low limits of detection (morphine 2.1 and oxymorphone 1.5 ng mL-1) and quantification (morphine 7.2 and oxymorphone 5.2 ng mL-1) in the EBC samples. The method had proper repeatability, accuracy, and stability expressed as relative standard deviations less than 5.1, 9, and 9%, respectively. The developed method was successfully used to determine morphine and oxymorphone concentrations in the EBC samples of addict patients.

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