Ultrasound-assisted Dispersive Solid-phase Microextraction Research Articles

A novel block copolymer containing gadolinium oxide nanoparticles in ultrasound assisted-dispersive solid phase microextraction of total arsenic in human foodstuffs: A multivariate optimization methodology

A new poly(3-hydroxy butyrate)-b-poly(dimethyl amino ethyl methacrylate) amphiphilic block copolymer containing gadolinium oxide nanoparticles (PHB-PDMAEMA-Gd2O3-NPs) were synthesized and used as composite adsorbent for extraction of total arsenic. Characterization of the composite adsorbent material PHB-PDMAEMA-Gd2O3-NP was studied using spectroscopic techniques. Plackett-Burman design and central composite design were employed to screening and optimization of the experimental parameters. This composite adsorbent was utilized in ultrasound assisted-dispersive solid phase microextraction (UA-dSPµE) for the determination of total inorganic arsenic in foodstuffs through hydride generation atomic absorption spectrometry (HG-AAS). It demonstrates a linear relationship across arsenic concentration range of 0.07–1.12 µg/L with a correlation coefficient (0.996). It’s showed an enrichment factor of 128 and a limit of detection 0.02 µg/L for total inorganic arsenic determination. Accuracy of the developed method was confirmed through the analysis of certified reference materials with 96.0–98.5% recovery. It proved to be significantly useful UA-dSPµE method for determining total inorganic arsenic in different foodstuffs.

Development of microextraction methods for the determination of sulfamethoxazole in water and biological samples: modelling, optimization and verification by central composite design

This study aimed to preconcentration of sulfamethoxazole (SMX) in water and biological samples. Ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and ultrasound-assisted dispersive solid-phase microextraction (UA-DSPME) methods paired with spectrophotometry were applied to extraction and preconcentration of SMX. ZnFe2O4 nanoparticles were prepared as adsorbent in UA-DSPME method by hydrothermal method. The scanning electron microscopy (SEM) technique showed that the adsorbent had symmetrical, bullet-shaped particles with uniform size. The results of the X-ray diffraction (XRD) showed the successful synthesis of the ZnFe2O4 nanoparticles. Effective parameters in extraction, including ultrasonication time, disperser solvent volume, adsorbent amount, extraction solvent volume, eluent volume, and pH were investigated and optimized. The practical and optimal conditions of the process were determined by the central composite design (CCD). The optimal conditions were 0.024 g of adsorbent, 535 µL of disperser solvent volume, 7.5 min of ultrasonication time, 235 µL of eluent volume, pH of 5, and 185 µL of extraction solvent volume. Linear ranges and detection limits were 20–1,200 μg L−1 and 6 μg L−1 for UA-DSPME and 10–800 μg L−1 and 3 μg L−1 for UA-DLLME. Relative standard deviation (RSD) of less than 4% were obtained for UA-DSPME and UA-DLLME methods. The reusability showed that the ZnFe2O4 adsorbent could extract SMX up to five cycles of adsorption/desorption without significant reduction in its efficiency. Also, interference studies showed that the presence of different cations and anions did not significantly interfere in the extraction of SMX. The outcomes of real-time samples analysis showed that the extraction of SMX for both methods was in the range of 92.44%–99.12%. The results showed the developed methods are simple, sensitive, and suitable for SMX preconcentration in environmental water and biological samples.

Ultrasound assisted dispersive solid phase microextraction using polystyrene-polyoleic acid graft copolymer for determination of Sb(III) in various bottled beverages by HGAAS

A new polyoleic acid-polystyrene (PoleS) block/graft copolymer was synthesized and applied as adsorbent for ultrasound assisted dispersive solid phase microextraction (UA-DSPME) of Sb(III) in different bottled beverages and analysis using hydride generation atomic absorption spectrometry (HGAAS). Adsorption capacity of the PoleS was 150 mg g−1. Several sample preparation parameters such as sorbent amount, solvent type, pH, sample volume and shaking time were optimized (based on central composite design (CCD) approach) and evaluated in respect to the recovery of Sb(III). The method revealed a high tolerance limit of matrix ions presence. Under optimized conditions, linearity range, the limit of detection, the limit of quantitation, extraction recovery, enhancement factor, preconcentration factor were 5–800 ng L−1, 1.5 ng L−1, 5.0 ng L−1, 96%, 82, 90, respectively. Accuracy of the UA-DSPME method was confirmed based on different certified reference materials and standard addition method. Factorial design was utilized to estimate the influences of variables of recovery of Sb(III).

An immobilization of aminopropyl trimethoxysilane-phenanthrene carbaldehyde on graphene oxide for toluene extraction and separation in water samples

A new functionalized Nano graphene with aminopropyl trimethoxysilane-phenanthrene-4-carbaldehyde (NGO@APTMS-PNTCA) as a novel adsorbent was used to extract toluene from water samples by the ultrasound-assisted dispersive solid-phase microextraction procedure (USA-D-SPME). So, 50 mg of NGO@APTMS-PNTCA adsorbent was added to water samples and sonicated for 20 min. After toluene extraction, the NGO@APTMS-PNTCA adsorbent separated from the liquid phase with a Whatman membrane filter (200 nm). Then, the toluene was back-extracted from the adsorbent by 2.0 mL of the acetone/ethanol (1:1, eluent) at 25 °C. Due to the physical properties and structure of toluene, fluorobenzene was used as an internal standard. Finally, the toluene values were measured by a gas chromatography-flame ionization detector (GC-FID). In optimized conditions, the limit of detection (LOD), the working range (WR), and the enrichment factor (EF) were obtained at 2.5 μg L−1, 0.01–1.2 mg L−1, and 9.63, respectively (MRSD% = 3.38). Also, the limit of quantification (LOQ) 10 μg L−1 and extraction recovery of more than 95% was efficiently achieved for toluene. Standard additions of toluene to blank solutions had high recoveries between 95.2% and 104.5% with a relative standard deviation (RSD%) of 0.27–5.2. The absorption capacities of NGO and NGO@APTMS-PNTCA adsorbents for toluene extraction were obtained at 32.8 mg g−1 and 154.9 mg g−1, respectively. The USA-D-SPME method was validated by spiking the standard concentrations of toluene. The proposed method demonstrated relevant and suitable statistical results with high accuracy and precision for toluene extraction by a novel adsorbent synthesis.

Nanostructured magnetic graphene oxide/UIO-66 sorbent for ultrasound-assisted dispersive solid-phase microextraction of food colorants in soft drinks, candies, and pastilles prior to HPLC analysis

Direct quantitative determination of food colorants in commercial food products is challenging due to their trace concentration. In this work, the magnetic graphene oxide/UIO-66 sorbent was used in an ultrasound-assisted dispersive solid-phase micro-extraction (UA-DSPME) process for the pre-concentration of Tartrazine (TA), Sunset Yellow (SY), and Allura Red (AR) food colorants prior to their quantitative determination using high-performance liquid chromatography (HPLC) analysis. Plackett-Burman design (PBD) was used to statistically explore all extract independent variables, and response surface methodology (RSM) was used to optimize the key variables. Under ideal circumstances, the method showed superior analytical performance with limits of detection (LOD) less than 0.070, 0.281, and 0.150 ng mL−1, and limits of quantitation (LOQ) less than 2.318, 9.368, and 4.988 ng mL−1 for TA, SY, and AR colorants, respectively. Furthermore, the procedure was effectively implemented with an extraction time of 15 min per sample with recoveries ranging from 95.01 to 106.33 %. Analysis of the standard reference material and recovery trials (>95 % relative recovery with lower than 6 % relative standard deviations) after spiking a known quantity of analyte in actual samples were used to evaluate the developed method's accuracy. The current method's distinctive benefits include minimal extraction time, high recovery, acceptable limit of detection, high accuracy, and good reusability in the development of pre-concentration and quantitative measurement of food colorants at trace levels in commercial food items.

Cellulose-based nanocomposite for ultrasonic assisted dispersive solid phase microextraction of triazole fungicides from water, fruits, and vegetables samples

Herein, an ultrasound-assisted dispersive solid phase microextraction (UA-DSPME) approach has been described for trace level analysis of triazole fungicides in real samples. For this purpose, a new nanosorbent was prepared through modification of carboxymethylcellulose biopolymer with zinc-based metal–organic framework and graphene oxide, and fully characterized. Then, the effect of extraction parameters on extraction efficiency was optimized for the microextraction process. Finally, desorbed triazole fungicides with ethanol were determined using gas chromatography equipped with flame ionization detector. This technique provided good linearity (R2 > 0.99), low detection limits (0.3–1.5 ng mL−1), high preconcentration factors (419–426), good relative recoveries (91.6–102 %), and high repeatability (RSD < 4.1 %) at optimized conditions (amount of sorbent: 15 mg; pH of solution: 7.0; and extraction time; 4 min). Ultimately, this approach was applied to determine triazole fungicides in different water and food samples.

Ultrasound-assisted dispersive micro-solid phase extraction of Pb(II) in water samples with in situ synthesis of magnetic Fe3O4-PbS nanocomposites followed by electrothermal atomic absorption spectrometry determination

Herein, an ultrasound-assisted dispersive magnetic micro-solid phase extraction (DM-μSPE) approach, along with electrothermal atomic absorption spectrometry (ETAAS) for the determination of lead at trace level in spring, well, river mineral and tap water samples was developed. The extraction step is based on the synthesis of PbS, following the sonochemical decomposition of L-cysteine used as sulphide precursor and its anchoring onto bare magnetite nanoparticles yielding the Fe3O4@PbS nanocomposite. Overall, DM-μSPE with in situ precipitation of PbS and retention onto magnetic sorbent requires a time as short as 6 min. After trapping Pb(II) as PbS, the magnetic nanocomposite was easily separated from the aqueous matrix by applying an external magnetic field and analyzed by ETAAS following slurry sampling. Different parameters involved in both the sorbent preparation/extraction and Pb quantification were optimized. Under optimal conditions, the method showed a detection limit of 0.02 μg L−1 Pb and a quantification limit of 0.07 μg L−1 Pb. The repeatability, expressed as relative standard deviation was 2% (for 0.6 μg L−1; n = 3). An experimental enrichment factor of 79 and an extraction efficiency of 99% were obtained. Finally, the method was applied for the determination of ultratrace levels of Pb(II) in spring, well, river mineral and tap water samples, showing quantitative recoveries in the range of 95–100%.

An adsorbent composed of alginate, polyvinylpyrrolidone and activated carbon (AC@PVP@alginate) for ultrasound-assisted dispersive micro-solid phase extraction of nevirapine and zidovudine in environmental water samples

In this study, AC@PVP@Alginate adsorbent synthesized using a facile cross-linking method was characterized using various techniques. The scanning electron microscopy and N2-adsorption/desorption analysis results confirmed that the synthesized nanocomposite was porous with a large specific surface area of 372 m2 g−1. The porous structure, a large surface area and multiple functional groups make the adsorbent suitable for efficient adsorption of target analytes. The adsorbent was applied in an ultrasonic-assisted dispersive micro-solid phase extraction for determining trace nevirapine and zidovudine in environmental water samples prior to high-performance liquid chromatography equipped with diode array detector analysis. Response surface methodology based on central composite design was applied for experimental parameters optimization. Under optimum experimental conditions, the method exhibited relatively acceptable intra-day precision, expressed as relative standard deviation, of ≤4.8%, low detection limits (LOD) and quantification limits (LOQ) ranging from 0.20 to 0.23 μg L−1 and 0.67–0.75 μg L−1, respectively. A spike recovery approach was used to assess the method applicability to real water samples and satisfactory relative recoveries ranging from 91.6 to 99.1% were obtained. The analysis of real water samples confirmed the presence of both analytes with maximum concentrations of 1.72 μg L−1 in influent wastewater.

Fe3O4@PDA@PANI core–shell nanocomposites as a new adsorbent for simultaneous preconcentration of Tartrazine and Sunset Yellow by ultrasonic-assisted dispersive micro solid-phase extraction

In this research, novel magnetic Fe3O4@PDA@PANI core–shell nanoparticles were designed and fabricated as an efficient adsorbent in the service of ultrasound-assisted dispersive micro-solid phase extraction for simultaneous preconcentration of Sunset Yellow (SY) and Tartrazine (Tar) before UV–Vis spectrophotometric detection. This adsorbent was fully characterized by Fourier Transform Infrared (FT-IR) spectroscopy, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Energy Dispersive X-ray (EDX) analysis. To overcome the spectral overlapping of SY and Tar dyes, the derivative spectrophotometric method was successfully used for the simultaneous detection of dyes in their binary solutions. The operating parameters affecting preconcentration efficiency and spectrophotometric determination were optimized. Under optimal conditions, the limit of detections (LOD) was obtained 0.2 and 0.5 ng mL−1 for SY and Tar, respectively. The adsorption capacity and reusability of core–shell nanoparticles were significant. The satisfactory results of analysis of a few real samples indicate that the method is very favored in the analysis of various complex matrices.

Ultrasound-assisted dispersive microsolid-phase extraction approach for preconcentration of trace cobalt and nickel and sensitive determination in water, food and tobacco samples by flame atomic absorption spectrometry

ABSTRACT Simpleand validated ultrasound-assisted dispersive microsolid-phase extraction (UA-DMSPE) approach for separation, and preconcentration of trace cobalt (Co(II)) and nickel (Ni(II)) ions in various water, juice, food and tobacco samples prior to their flame atomic absorption spectrometry determination (FAAS) was developed. The proposed method based on using oxidized multiwalled carbon nanotubes (ox-MWCNTs) as adsorbent and 3-(2-hydroxy-5-acetylphen-1-ylazo)-1,2,4-triazole (HAPAT) as complexing agent at pH 7.0. The effect of different parameters has been investigated and optimised. The calibration curves were linear in the ranges of 1.0–300 and 2.0–400 μg L−1 and the limits of detection were 0.30 and 0.60 μg L−1 for Co(II) and Ni(II) ions, respectively, under the optimum conditions.The preconcentration factor was 200. Co(II) and Ni(II) havemaximum sorption capacities of around 300 and 370 mg g–1, respectively. The recovery rates of the analytes ranged from 96.0 to 101%. Furthermore, relative standard deviation (RSD%) for intra-day (1.40 and 1.90%) and inter-day (1.70 and 2.10%) as repeatability for Co(II) and Ni(II), respectively. Certified reference materials (SRM 1570A spinach leaves and TMDA-52.3 fortified water) were used to verify the accuracy of the proposed preconcentration protocol. The proposed method was successfully used to determine the content of Co(II) and Ni(II) ions in a variety of real water, juice, food and tobacco samples yielding satisfactory results.

Reduced Graphene Oxide-Cadmium Sulfide Quantum Dots Nanocomposite Based Dispersive Solid Phase Microextraction for Ultra-Trace Determination of Carbamazepine and Phenobarbital

This research presents a fast, sensitive, and selective ultrasound-assisted dispersive solid phase microextraction technique for simultaneous preconcentration and determination of ultra-trace amount of carbamazepine and phenobarbital. Reduced graphene oxide sheets decorated with cadmium sulfide quantum dots was synthesized, characterized, and used as a high capacity adsorbent. A high performance liquid chromatography with UV detector (HPLC-UV) instrument with 58:42 composition of methanol:acetic acid/acetate buffer (pH = 5; 0.05 mol L-1) as the mobile phase and set on the wavelength of 230 nm was used to separate and quantify the analytes. In this regard, different parameters affecting adsorption and desorption of the analytes on the surface of the nanocomposite were studied and optimized to maximize the efficiency of the method. The method was linear in the ranges of 0.5-180 and 0.5-140 ng mL−1 (correlation coefficient (r) &gt; 0.999) with limits of detection of 0.19 and 0.24 ng mL−1 for carbamazepine and phenobarbital, respectively. Eventually, to evaluate the efficiency of the proposed method for the determination of pharmaceuticals in biological samples, different real samples including breast milk, urine and human plasma were tested. Obtained recoveries values were within the range of 96.3 ± 2 to 103.7 ± 3.3% which showed satisfactory efficiency.

Dispersive solid phase extraction using graphitic carbon nitride microparticles for the determination of trace amounts of lead in water samples

In this work, ultrasound-assisted dispersive micro-solid phase extraction (USA-D-µSPE) technique using graphitized carbon nitride (g-C3N4) is proposed for the preconcentration of low level of lead in aqueous samples. In this method, microparticles of graphitized carbon nitride sorbent were dispersed in the samples using ultrasonic bath and Pb(II) ions were directly adsorbed on the surface of g-C3N4 particles. After adsorption and desorption of lead ions from g-C3N4 particles, the Pb concentration was determined by the inductively coupled plasma- optical emission spectroscopy (ICP-OES). The main advantages of this method are high speed, simplicity and cheapness. The effects of pH, sorbent amount, eluent type and time on the recovery of the analyte were investigated. Under the optimized conditions and preconcentration of 10 mL of sample, the detection limit of 1.24 μg L-1 was obtained. The results were validated by standard reference materials (NIST, SRM) and spiking of real samples by USA-D-µSPE procedure.

Ultrasound assisted dispersive solid phase microextraction of inorganic arsenic from food and water samples using CdS nanoflowers combined with ICP-OES determination

Direct determination of arsenic species in real samples is challenging due to their trace concentration and spectral interferences by coexisting ions. Herein, we proposed an ultrasound-assisted dispersive solid phase microextraction (DSPME) procedure for the analyses of the trace inorganic arsenic. The hydrothermally synthesized cadmium sulfide nanoparticles (CdS NPs) completely adsorbed both arsenic species within 20 s at the initial arsenic concentration of 100 µg L−1. The detection limit (3 S/m) of the proposed method was found to be 0.5 ± 0.2 and 0.8 ± 0.2 ng L−1 for As(III) and As(V), respectively. The accuracy of the method against the systematic and constant errors was confirmed by the analysis of the Standard Reference Material (SRM) (>95% recovery with <5% RSD). The Student’s t-test values were found to be less than the critical Student’s t value at a 95% confidence level. The method was successfully employed for the determination of arsenic in food samples.

Ultrasound-assisted dispersive micro-solid phase extraction using molybdenum disulfide supported on reduced graphene oxide for energy dispersive X-ray fluorescence spectrometric determination of chromium species in water

Molybdenum disulfide (MoS2) was supported on graphene oxide (GO) by hydrothermal method. The resulting nanocomposite (MoS2-rGO) was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy. The experiments show that at pH 2, MoS2-rGO has a great affinity for adsorption of hexavalent chromium ions while Cr(III) ions remain in aqueous sample. In the adsorption process, the dominant role plays chemisorption. The determined adsorption capacity is 583.5 mg g−1. Parameters affecting the extraction process, namely sample pH, sample volume, contact time, and matrix ions, were investigated by sequential batch tests. Under optimal conditions (pH 2, sample volume 50 mL, sonication time 10 min, adsorbent mass 1 mg), the calibration curve covers the 1–200 ng mL−1 range with a correlation coefficient (R2) of 0.998. The recovery of the method is 97 ± 3%. Other data of merit include a relative standard deviation of < 3.5%, enrichment factor of 3350, and detection limit of 0.050 ng mL−1. The accuracy of the method was confirmed by analysis of the reference materials QC1453 (chromium VI in drinking water) and QC3015 (chromium VI in seawater). The method was successfully applied to chromium speciation in water samples, including high salinity ones. The concentration of Cr(III) was calculated as the difference between the total concentration of chromium (after oxidation of Cr(III) to Cr(VI) with potassium permanganate) and the initial Cr(VI) content.Graphical abstractSchematic presentation of a method for determination of chromium species by energy dispersive X-ray fluorescence spectrometry after preconcentration on molybdenum disulfide supported on reduced graphene oxide.

On-line ultrasound-assisted dispersive micro-solid phase extraction using graphitic carbon nitride microparticles combined with ICP-OES for the preconcentration and determination of thorium

In this study, on-line ultrasound-assisted dispersive micro-solid phase extraction technique is introduced for the separation and ICP-OES determination of thorium in aqueous samples. In this method, microparticles of g-C3N4 were dispersed into the sample using ultrasonic radiation and Th(IV) ions were directly adsorbed by the sorbent. The sample solution was then passed through a membrane filter and the adsorbed Th(IV) ions were subsequently eluted directly into the ICP-OES nebulizer. The Limit of detection of developed method was 0.05 μg L−1. The developed on-line technique eliminates the centrifugation step in order to simplify and speed up the extraction procedure.

Ultrasound-assisted dispersive solid-phase microextraction of capecitabine by multi-stimuli responsive molecularly imprinted polymer modified with chitosan nanoparticles followed byHPLC analysis.

An ultrasonic-assisted dispersive solid-phase microextraction was developed by a multi-stimuli responsive molecularly imprinted polymer based on chain transfer agent-modified chitosan nanoparticles for enrichment and separation of trace capecitabine in a real sample. The synthesized particles were carefully characterized and it wasfound that a uniform pH-sensitive imprinted polymeric shell isobtained on the surface of Fe3O4@chitosan core with enough saturation magnetization (29emug-1). Desirable adsorption capacity (91mgg-1) and high imprinting factor (IF = 3.6) toward capecitabine were exhibited by the Langmuir isotherm model. Under optimized conditions, which wereachieved by experimental design, the detection limit (S/N = 3) was 1.9ngmL-1. The obtained relative mean recoveries of capecitabine using high-performance liquid chromatography were in the range of 93 to 102% in a human plasma sample with RSD less than 5.5%. Graphical abstract Schematic representation of ultrasonic-assisted dispersive solid-phase microextraction by multi-stimuli responsive molecularly imprinted polymer based on chain transfer agent-modified chitosan nanoparticles and high-performance liquid chromatography for enrichment and separation of capecitabine in the real sample.

Development of ultrasound-assisted dispersive solid-phase microextraction based on mesoporous carbon coated with silica@iron oxide nanocomposite for preconcentration of Te and Tl in natural water systems

Abstract The main objective of this study was to develop an ultrasound-assisted dispersive solid-phase microextraction (UADSPME) method for separation and preconcentration of tellurium (Te) and thallium (Tl) in environmental samples prior to inductively coupled plasma-optical emission spectrometry determination. The MPC@SiO2@Fe3O4 nanocomposite was used as a nanoadsorbent in the UADSPME method. The nanocomposite was prepared using a coprecipitation and sol–gel method, and it was characterized using scanning electron microscopy/energy-dispersive X-ray spectroscopy, transmission electron microscopy and X-ray powder diffraction techniques. The Box–Behnken design and response surface methodology were used for the optimization of experimental parameters (such as pH, extraction time and mass of adsorbent) affecting the preconcentration procedure. Under optimized conditions, the limits of detection were 0.05 and 0.02 µg L−1 and the limits of quantification were 0.17 and 0.07 µg L−1 for Te and Tl, respectively. The precision expressed as the relative standard deviation (%RSD) was 2.5% and 2.8% for Te and Tl, respectively. Finally, the developed method was applied for the analysis of Tl and Te in real samples.

MgO-ZnO/carbon nanofiber nanocomposite as an adsorbent for ultrasound-assisted dispersive solid-phase microextraction of carbamazepine from wastewater prior to high-performance liquid chromatographic detection

A simple, rapid, and efficient ultrasound-assisted dispersive solid-phase microextraction (UA-DSPME) method was developed for the preconcentration of carbamazepine (CBZ) in wastewater prior to high-performance liquid chromatography coupled with diode array (HPLC-DAD) determination. The carbon nanofibers coated with magnesium oxide-zinc oxide (MgO-ZnO@CNFs) nanocomposite was used as an efficient adsorbent in magnetic dispersive solid-phase microextraction method. The structural and morphological properties of the nanocomposite were characterized by scanning electron microscopy and energy dispersive spectroscopy, transmission electron microscopy, X-ray diffractometer, and Fourier transform infrared spectroscopy. The surface area was investigated using Brunauer–Emmett–Teller. Several factors (such as pH, mass of adsorbent, extraction time, and eluent volume) that affect extraction and preconcentration of CBZ were also assessed and optimized using response surface methodology based on central composite design. Under optimal conditions, the limits of detection (LOD) and quantification were 0.08 μg L−1 and 0.29 μg L−1, respectively. The calibration curve constructed after preconcentration of seven successive standards was linear in the concentration range of 0.3–800 μg L−1 with the correlation coefficient of 0.9922. The intra-day and inter-day precisions expressed in terms of relative standard deviation were 1.4% and 4.2%. A preconcentration factor of 490 was achieved, and the method was applied for the analysis of spiked wastewater. Satisfactory recoveries ranging from 97.8 to 102% were obtained.

Ultrasonically synthesis of Mn- and Cu- @ ZnS-NPs-AC based ultrasound assisted extraction procedure and validation of a spectrophotometric method for a rapid preconcentration of Allura Red AC (E129) in food and water samples

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 < 3.5%, which demonstrate the successful applicability of present method for real sample analysis. The maximum sorbent capacity was 50.0 mg g−1 based on Langmuir isotherm as best model with high correlation coefficient. Combination of UA-DSPME and UV–Vis lead to higher sensitivity and lower cost for accurate and repeatable monitoring of Allura Red level in beverage, fruit juice and drink water samples with acceptable recovery and reasonable RSD%.

Determination of β-carotene and total carotenoids in fruit juices using surfactant surface decorated graphene oxide based ultrasound-assisted dispersive solid-phase microextraction

In this study, the influence of surfactants (SDS, TX100 and CTAB) to modify surface polarity of graphene oxide adsorbent is proposed for the extraction of β-carotene and total carotenoids from fruit juice samples.