A simple and efficient sequential electrokinetic and hydrodynamic injections in micellar electrokinetic chromatography method for quantification of anticancer drug 5-fluorouracil and its metabolite in human plasma.

A simple and sensitive preconcentration strategy using sequential electrokinetic and hydrodynamic injection modes in micellar electrokinetic chromatography with diode array detection was developed and applied for the separation and determination of anticancer agent, 5-fluorouracil and its metabolite, 5-fluoro-2'-deoxyuridine, in human plasma. Sequential injection modes with increased analyte loading capacity using the anionic pseudo-stationary phase facilitated collection of the dispersed neutral and charged analytes into narrow zones and improved sensitivity. Several important parameters affecting sample enrichment performance were evaluated and optimized in this study. Under the optimized experimental conditions, 614- and 643-fold and 782- and 803-fold sensitivity improvement were obtained for 5-fluorouracil and its metabolite when compared with normal hydrodynamic and electrokinetic injection, respectively. The method has good linearity (1-1,000 ng/ml) with acceptable coefficient of determination (r2 > 0.993), low limits of detection (0.11-0.14 ng/ml) and satisfactory analyte relative recovery (97.4-99.7%) with relative standard deviations of 4.6-9.3% (n = 6). Validation results as well as the application to analysis of human plasma samples from cancer patients demonstrate the applicability of the proposed method to clinical studies.

Electrochemically Modulated Liquid-Liquid Extraction for Sample Enrichment.

A new sample preparation method is proposed for the extraction of pharmaceutical compounds (Metformin, Phenyl biguanide, and Phenformin) of varied hydrophilicity, dissolved in an aqueous sample. When in contact with an organic phase, an interfacial potential is imposed by the presence of an ion, tetramethylammonium (TMA+), common to each phase. The interfacial potential difference drives the transfer of ionic analytes across the interface and allows it to reach up to nearly 100% extraction efficiency and a 60-fold enrichment factor in optimized extraction conditions as determined by HPLC analysis.

Determination of Biogenic Amines in Seawater Using Capillary Electrophoresis with Capacitively Coupled Contactless Conductivity Detection.

A rapid and green analytical method based on capillary electrophoresis with capacitively coupled contactless conductivity detection (C4D) for the determination of eight environmental pollutants, the biogenic amines (putrescine, cadaverine, spermidine, spermine, tyramine, 2-phenylamine, histamine and tryptamine), is described. The separation was achieved under normal polarity mode at 24 °C and 25 kV with a hydrodynamic injection (50 mbar for 5 s) and using a bare fused-silica capillary (95 cm length × 50 µm i.d.) (detection length of 10.5 cm from the outlet end of the capillary). The optimized background electrolyte consisted of 400 mM malic acid. C4D parameters were set at a fixed amplitude (50 V) and frequency (600 kHz). Under the optimum conditions, the method exhibited good linearity over the range of 1.0⁻100 µg mL−1 (R² ≥ 0.981). The limits of detection based on signal to noise (S/N) ratios of 3 and 10 were ≤0.029 µg mL−1. The method was used for the determination of seawater samples that were spiked with biogenic amines. Good recoveries (77⁻93%) were found.

Evaluation of extraction methods for the identification of proteins from date palm (Phoenix dactylifera L.) seed and flesh.

Date fruits are well known to be very nutritious. Nevertheless, the protein contents of the fruit, particularly the seed and flesh, are still understudied, largely due to their difficult physical characteristics. This study was conducted to compare three different protein extraction methods which were the trichloroacetic acid (TCA)-acetone (TCA-A), phenol (Phe), and TCA-acetone-phenol (TCA-A-Phe), and to perform proteomic analysis on date palm seed and flesh. Phe extraction method showed the highest protein yields for both seed (8.26 mg/g) and flesh (1.57 mg/g). Through sodium dodecyl sulfate-polyacrylamide gel electrophoresis, Phe, and TCA-A-Phe extraction methods were shown to be efficient in removing interfering compounds and gave well-resolved bands over a wide range of molecular weights. Following liquid chromatography-tandem mass spectrometry analysis, about 50-64% of extracted proteins were identified with known functions including those involved in glycolysis, Krebs cycle, defense, and storage. Phe protein extraction method was proven to be the optimal method for date flesh and seed.

Vortex- and CO2 -gas-assisted liquid-liquid microextraction with salt addition for the high-performance liquid chromatographic determination of furanic compounds in concentrated juices and dried fruits.

A novel microextraction method based on vortex- and CO2 -assisted liquid-liquid microextraction with salt addition for the isolation of furanic compounds (5-hydroxymethyl-2-furaldehyde, 5-methyl-2-furaldehyde, 2-furaldehyde, 3-furaldehyde, 2-furoic and 3-furoic acids) was developed. Purging the sample with CO2 was applied after vortexing to enhance the phase separation and mass transfer of the analytes. The optimum extraction conditions were: extraction solvent (volume), propyl acetate (125 µL); sample pH, 2.4; vortexing time, 45 s; salt concentration, 25% w/v and purging time, 5 min. The analytes were separated using an ODS Hypersil C18 column (250×4.6 mm i.d, 5 µm) under gradient flow. The proposed method showed good linearities (r(2) >0.999), low detection limits (0.08-1.9 µg/L) and good recoveries (80.7-122%). The validated method was successfully applied for the determination of the furanic compounds in concentrated juice (mango, date, orange, pomegranate, roselle, mangosteen and soursop) and dried fruit (prune, date and apricot paste) samples.

Development of ß-cyclodextrin crosslinked citric acid encapsulated in polypropylene membrane protected-µ-solid-phase extraction device for enhancing the separation and preconcentration of endocrine disruptor compounds.

Endocrine disruptor compounds (EDCs) such as plasticisers, surfactants, pharmaceutical products, personal care products and pesticides are frequently released into the environmental waters. Therefore, a sensitive and environmentally friendly method is entailed to quantify these compounds at their trace level concentrations. This study encapsulated the ß-cyclodextrin crosslinked with citric acid in a polypropylene membrane protected-µ-solid phase extraction (BCD-CA µ-SPE) device for preconcentrating the EDCs (triclosan, triclocarban, 2-phenylphenol, 4-tert-octylphenols and bisphenol A) in real water samples before the analysis by high-performance liquid chromatography. FT-IR and TGA results indicated that BCD-CA was successfully synthesised with the formation of ester linkage (1078.33 cm-1) and O-H stretching from carboxylic acid (3434.70 cm-1) with higher thermal stability as compared with native CD with the remaining weight above 72.1% at 500 °C. Several critical parameters such as the sorbent loading, type and amount of salts, extraction time, sample volume, sample pH, type and volume of desorption solvents and desorption time were sequentially optimised and statistically validated. Under the optimum condition, the use of BCD-CA µ-SPE device had manifested good linearity (0.5-500 µg L-1) with the determination of the coefficient range of 0.9807-0.9979. The p-values for the F-test and t-test (6.60 × 10-8 - 1.77 × 10-5) were lesser than 0.05 and low detection limits ranging from 0.27 to 0.84 µg L-1 for all studied EDCs. The developed technique was also successfully applied for EDC analyses in four distinct real water samples, namely, wastewater, river water, tap water and mineral water, with good EDCs recoveries (80.2%-99.9%), low relative standard deviations (0.1%-3.8%, n = 3) with enrichment factor ranging from 9 to 82 folds. These results signified the potential of the BCD-CA µ-SPE device as an efficient, sensitive, and environmentally friendly approach for analyzing EDCs.

Induced sample via transient isotachophoresis mediated with sweeping in micellar electrokinetic chromatography for the dual-stacking strategy of non-steroidal anti-inflammatory drugs in environmental water samples.

Realising the need to devise a simple, sensitive, and reliable detection method, this study investigated the development of a dual-stacking transient isotachophoresis (t-ITP) and sweeping in micellar electrokinetic chromatography with diode array detector (t-ITP/sweeping-MEKC-DAD) for the determination of selected non-steroidal anti-inflammatory drugs (NSAIDs); ketoprofen, diclofenac and naproxen from aqueous matrices. Prior to the system setup, various parameters were optimised to assess the potential use of the t-ITP paired with the sweeping stacking technique in micellar background electrolyte for dual preconcentration and separation of trace amounts of NSAIDs. Once the optimum conditions have been established, the method performance was validated and applied to 17 environmental water samples. Based on the results, the combined t-ITP and sweeping approach significantly improved the stacking and separation sensitivity. A large volume of samples could also be introduced and subsequently separated by MEKC with greater focusing effects due to the sweeping. Under optimised conditions, the developed method exhibited excellent linearity at a high range (0.1-500 ng/mL, r2 ≥ 0.998), low limits of detection (LODs) of 0.01-0.07 ng/mL, and a remarkable relative recovery (RR) of 99.6-101.9% with a relative standard deviation (RSD) of 1.4-8.6% (n = 9). Ultimately, the sensitivity enhancement factors improved up to 666-fold using the optimised method. Therefore, the proposed method presents a simplified yet effective and suitable for the determination of NSAIDs from aqueous matrices.

Competitive removal mechanism to simultaneously incarcerate bisphenol A, triclosan and 4-tert-octylphenol within beta-cyclodextrin crosslinked citric acid used for encapsulation in polypropylene membrane protected-micro-solid-phase extraction.

Endocrine disrupting compounds (EDCs) are extensively found in the environment and severely impacting human health. In addressing this issue, the beta-cyclodextrin crosslinked citric acid (BCD-CA) had been previously employed in membrane-protected micro-solid phase extraction for sequestering EDCs from water medium; and the findings revealed that BCD-CA possessed a selectivity property. On that account, the potential of BCD-CA towards competitive adsorption of selected EDCs was investigated in terms of adsorption mechanism and selectivity property. Factors that affected the removal efficiencies such as sample pH, sorbent dosage, contact time and initial concentration were evaluated. The characterization results revealed that the carbon percentage of BCD-CA had increased by 2.04%, while the hydrogen percentage had reduced by 1.83%, signifying the successful crosslinking of BCD-CA. Besides, the amount of active BCD was calculated to be 3.2 × 10-7 mol, while the amount of carboxyl group was 2.48 × 10-5 mol per 4 mg of BCD-CA. Moreover, BCD-CA was stable in an aqueous medium with the zeta potential obtained at -36.5 mV and had a high-water retention capacity (∼150%). The competitive adsorption mechanism by BCD-CA with EDCs followed the pseudo-second-order kinetics and Freundlich isotherm, suggesting that the adsorption process was dominated by chemisorption on the heterogeneous surface of the adsorbent. Thermodynamic results revealed that adsorption of 4-tert-octylphenol had the most negative ΔG value, indicating most favorable to be adsorbed by BCD-CA as opposed to triclosan and bisphenol A, which was coherent with the apparent formation constant results. These unique properties manifested the practicality of BCD-CA as a selective adsorbent to detect and remove EDCs from the water medium.

Simultaneous preconcentration and determination of sulfonamide antibiotics in milk and yoghurt by dynamic pH junction focusing coupled with capillary electrophoresis.

A dynamic pH junction was used in capillary electrophoresis (CE-DAD) to on-line preconcentrate, separate, and determine trace amounts of sulfonamide antibiotics (SAs) in milk and yoghurt samples in this study. A sample matrix with 0.15% acetic acid and 10% methanol (MeOH) at a pH of 4.0, and a background electrolyte (BGE) that contained 35 mM sodium citrate with 10% MeOH at a pH of 8.5, and an acidic barrage of 0.4% acetic acid with 10% MeOH at a pH of 2.5 were utilised to achieve a stacking effect for SAs through a dynamic pH junction. Under optimised conditions, the proposed preconcentration method showed good linearity (30-500 ng/mL, r2 ≥ 0.9940), low limits of detection (LODs) of 4.1-6.3 ng/mL, and acceptable analytes recovery (81.2-106.9%) with relative standard deviations (RSDs) within 5.3-13.7 (n = 9). The limits of quantification (LOQs) were below the maximum residue limit approved by the European Union (EU) in this type of matrices. Sensitivity enhancement factors of up to 129 were reached with the optimised dynamic pH junction using CE with a diode array detector (DAD). The method was used to determine SAs in fresh milk, low-fat milk, full-cream milk, and yoghurt samples.

Ionophore-based potentiometric sensors for the flow-injection determination of promethazine hydrochloride in pharmaceutical formulations and human urine.

Plasticised poly(vinyl chloride)-based membranes containing the ionophores (α-, ß- and γ-cyclodextrins (CD), dibenzo-18-crown-6 (DB18C6) and dibenzo-30-crown-10 (DB30C10) were evaluated for their potentiometric response towards promethazine (PM) in a flow injection analysis (FIA) set-up. Good responses were obtained when ß- and γ-CDs, and DB30C10 were used. The performance characteristics were further improved when tetrakis(4-chlorophenyl) borate (KTPB) was added to the membrane. The sensor based on ß-CD, bis(2-ethylhexyl) adipate (BEHA) and KTPB exhibited the best performance among the eighteen sensor compositions that were tested. The response was linear from 1 × 10(-5) to 1 × 10(-2) M, slope was 61.3 mV decade(-1), the pH independent region ranged from 4.5 to 7.0, a limit of detection of 5.3 × 10(-6) M was possible and a lifetime of more than a month was observed when used in the FIA system. Other plasticisers such as dioctyl phenylphosphonate and tributyl phosphate do not show significant improvements in the quality of the sensors. The promising sensors were further tested for the effects of foreign ions (Li(+), Na(+), K(+), Mg(2+), Ca(2+), Co(2+), Cu(2+), Cr(3+), Fe(3+), glucose, fructose). FIA conditions (e.g., effects of flow rate, injection volume, pH of the carrier stream) were also studied when the best sensor was used (based on ß-CD). The sensor was applied to the determination of PM in four pharmaceutical preparations and human urine that were spiked with different levels of PM. Good agreement between the sensor and the manufacturer's claimed values (for pharmaceutical preparations) was obtained, while mean recoveries of 98.6% were obtained for spiked urine samples. The molecular recognition features of the sensors as revealed by molecular modelling were rationalised by the nature of the interactions and complexation energies between the host and guest molecules.

Removal of 4-chloro-2-methylphenoxyacetic acid from water by MIL-101(Cr) metal-organic framework: kinetics, isotherms and statistical models.

Effective removal of 4-chloro-2-methylphenoxyacetic acid (MCPA), an emerging agrochemical contaminant in water with carcinogenic and mutagenic health effects has been reported using hydrothermally synthesized MIL-101(Cr) metal-organic framework (MOF). The properties of the MOF were ascertained using powdered X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermal gravimetric analysis (TGA), field emission scanning electron microscopy (FESEM) and surface area and porosimetry (SAP). The BET surface area and pore volume of the MOF were 1439 m2 g-1 and 0.77 cm3 g-1, respectively. Artificial neural network (ANN) model was significantly employed for the accurate prediction of the experimental adsorption capacity (qe ) values with minimal error. A rapid removal of the pollutant (99%) was recorded within short time (approx. 25 min), and the reusability of the MOF (20 mg) was achieved up to six cycles with over 90% removal efficiency. The kinetics, isotherm and thermodynamics of the process were described by the pseudo-second-order, Freundlich and endothermic adsorption, respectively. The adsorption process is spontaneous based on the negative Gibbs free energy values. The significant correlation between the experimental findings and simulation results suggests the great potential of MIL-101(Cr) for the remediation of MCPA from water matrices.

Graphene and zeolite as adsorbents in bar-micro-solid phase extraction of pharmaceutical compounds of diverse polarities.

A bar micro-solid phase (bar µ-SPE) extraction method using either graphene or zeolite or their mixtures as an adsorbent, coupled with high-performance liquid chromatography (using a C1 column) was developed for the simultaneous determination of pharmaceutical compounds (metformin (MET), buformin (BUF), phenformin (PHEN) and propranolol (PROP)) of diverse polarity (log P from -1.82 to 3.10). Parameters influencing the extraction, such as conditioning solvents, pH of the sample, sample volume, amount of adsorbent, stirring rate, time of extraction, type and volume of desorption solvent and time of desorption were investigated. Under the optimized conditions, the extraction method using graphene (extraction efficiency, % EE, ∼6-15%) resulted in the least amount of extracted drugs. However, the use of zeolite and zeolite/graphene mixtures improves the % EE significantly, i.e. 30% for PHEN and 42% for PROP using zeolite; 22% for MET and 18% for BUF using the adsorbent mixture. Under similar conditions, enrichment factors for these drugs range from 11-15. The validated method was performed for the determination of the drugs that were spiked to urine samples. Good recoveries ranging from 72.8 to 116% were achieved.

Determination of the binding constants of modafinil enantiomers with sulfated ß-cyclodextrin chiral selector by capillary electrophoresis using three different linear plotting methods.

Binding constants for the enantiomers of modafinil with the negatively charged chiral selector sulfated-ß-CD (S-ß-CD) using CE technique is presented. The calculations of the binding constants employing three different linearization plots (double reciprocal, X-reciprocal and Y-reciprocal) were performed from the electrophoretic mobility values of modafinil enantiomers at different concentrations of S-ß-CD in the BGE. The highest inclusion affinity of the modafinil enantiomers were observed for the S-enantiomer-S-ß-CD complex, in agreement with the computational calculations performed previously. Binding constants for each enantiomer-S-ß-CD complex at different temperatures, as well as thermodynamic parameters for binding, were calculated. Host-guest binding constants using the double reciprocal fit showed better linearity (r(2)>0.99) at all temperatures studied (15-30°C) and compared with the other two fit methods. The linear van't Hoff (15-30°C) plot obtained indicated that the thermodynamic parameters of complexation were temperature dependent for the enantiomers.

Simultaneous determination of atenolol, chlorthalidone and amiloride in pharmaceutical preparations by capillary zone electrophoresis with ultraviolet detection.

Capillary zone electrophoresis methods for the simultaneous determination of the beta-blocker drugs, atenolol, chlorthalidone and amiloride, in pharmaceutical formulations have been developed. The influences of several factors (buffer pH, concentration, applied voltage, capillary temperature and injection time) were studied. Using phenobarbital as internal standard, the analytes were all separated in less than 4 min. The separation was carried out in normal polarity mode at 25 degrees C, 25 kV and using hydrodynamic injection (10 s). The separation was effected in an uncoated fused-silica capillary (75 mum i.d. x 52 cm) and a background electrolyte of 25 mm H(3)PO(4) adjusted with 1 m NaOH solution (pH 9.0) and detection at 198 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 1-250 microg/mL for atenolol and chlorthalidone and from 2.5-250 microg/mL for amiloride. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of atenolol, chlorthalidone and amiloride in various pharmaceutical tablets formulations.

Simultaneous determination of atenolol and amiloride in pharmaceutical preparations by capillary zone electrophoresis with capacitively coupled contactless conductivity detection.

Capillary zone electrophoresis coupled with a capacitively coupled contactless conductivity detector (CE-C(4)D) has been employed for the determination of atenolol and amiloride in pharmaceutical formulations. Acetic acid (150 mm) was used as background electrolyte. The influence of several factors (detector excitation voltage and frequency, buffer concentration, applied voltage, capillary temperature and injection time) was studied. Non-UV-absorbing L-valine was used as internal standard; the analytes were all separated in less than 7 min. The separation was carried out in normal polarity mode at 28 degrees C, 25 kV and using hydrodynamic injection (25 s). The separation was effected in an uncoated fused-silica capillary (75 microm, i.d. x 52 cm). The CE-C(4)D method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 5-250 microg/mL for the studied analytes. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of atenolol and amiloride in different pharmaceutical tablet formulations.

Capillary electrophoretic separation and computational modeling of inclusion complexes of beta-cyclodextrin and 18-crown-6 ether with primaquine and quinocide.

The antimalarial drug primaquine (PQ) and its contaminant, the positional isomer quinocide (QC) have been successfully separated using capillary electrophoresis with either beta-cyclodextrin (beta-CD) or 18-crown-6 ether (18C6) as chiral mobile phase additive. The interactions of the drugs with cyclodextrins and 18C6 were studied by the semiempirical method (Parametric Model 3) PM3. Theoretical calculations for the inclusion complexes of PQ and QC with alpha-CD, beta-CD and 18C6 were performed. Data from the theoretical calculations are correlated and discussed with respect to the electrophoretic migration behavior. More stable complexes are predicted for the PQ-beta-CD and PQ-18C6 complexes. The coelution of PQ and QC when alpha-CD was used as buffer additive can be explained by their comparable stabilities of the inclusion complex formed, while significant differences in the complexation stabilities of the drugs with beta-CD is responsible for their separation. The stronger hydrogen bonding in PQ-18C6 system is responsible for the separation between PQ and QC when 18C6 was used as chiral mobile phase additive.

Assay and stability-indicating micellar electrokinetic chromatography method for the simultaneous determination of valacyclovir, acyclovir and their major impurity guanine in pharmaceutical formulations.

A micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of the antiviral drugs acyclovir and valacyclovir and their major impurity, guanine, was developed. The influences of several factors (surfactant and buffer concentration, pH, applied voltage, capillary temperature and injection time) were studied. Using tyramine hydrochloride as internal standard, the analytes were all separated in about 4 min. The separation was carried out in reversed polarity mode at 28 degrees C, 25 kV and using hydrodynamic injection (15 s). The separation was effected in a fused-silica capillary 100 microm x 56 cm and a background electrolyte of 20 mM citric acid-1 M Tris solution (pH 2.75), containing 125 mM sodium dodecyl sulphate and detection at 254 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 0.1-1 microg/mL (guanine) and from 0.1 to 120 microg/mL for both valacyclovir and acyclovir. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 5.0%. The proposed method was successfully applied to the determination of the analytes in tablets and creams. From the previous study it is concluded that the stability-indicating method developed for acyclovir and valacyclovir can be used for analysis of the drug in various stability samples.

Adsorption of dicamba and MCPA onto MIL-53(Al) metal-organic framework: response surface methodology and artificial neural network model studies.

An aluminium-based metal-organic framework ((MOF), MIL-53(Al)), was hydrothermally synthesized, characterized and applied for the remediation of the herbicides dicamba (3,6-dichloro-2-methoxy benzoic acid) and 4-chloro-2-methylphenoxyacetic acid (MCPA) in aqueous medium. Response surface methodology (RSM) and artificial neural network (ANN) were used to design, optimize and predict the non-linear relationships between the independent and dependent variables. The shared interaction of the effects of key response parameters on the adsorption capacity were assessed using the central composite design-RSM and ANN optimization models. The optimum adsorption capacities for dicamba and MCPA are 228.5 and 231.9 mg g-1, respectively. The RSM ANOVA results showed significant p-values, with coefficients of determination (R 2) = 0.988 and 0.987 and R 2 adjusted = 0.974 and 0.976 for dicamba and MCPA, respectively. The ANN prediction model gave R 2 = 0.999 and 0.999, R 2 adjusted = 0.997 and 0.995 and root mean square errors (RMSEs) of 0.001 and 0.004 for dicamba and MCPA, respectively. In each set of experimental conditions used for the study, the ANN gave better prediction than the RSM, with high accuracy and minimal error. The rapid removal (∼25 min), reusability (5 times) and good agreement between the experimental findings and simulation results suggest the great potential of MIL-53(Al) for the remediation of dicamba and MCPA from water matrices.

Simultaneous Quantitative Assessment of Ochratoxin A, Patulin, 5-Hydroxymethylfurfural, and Bisphenol A in Fruit Drinks Using HPLC with Diode Array-Fluorimetric Detection.

The analysis of regulated contaminants in fruit drinks often requires suitable validated and rapid analytical methods for cost-effective food control, and is of considerable interest among the fruit beverage industry. This study demonstrated a rapid and sensitive high-performance liquid chromatography approach for the simultaneous determination of ochratoxin A (OTA), patulin (PAT), 5-hydroxymethylfurfural (HMF), and bisphenol A (BPA) in various fruit drinks. The separations were achieved using a C18 core-shell column with both photo-diode array and fluorimetric detections connected in series. A gradient system consisting of methanol and 0.1% formic acid at a flow rate of 1.2 mL min-1, thermostated at 35 °C, provided fast elution with run time <9 min. Sample pretreatment was optimised to enable extraction of all analytes from fruit drink matrices. The optimised method was validated. Correlation coefficients of R > 0.99 were achieved with detection limits of 0.5 ng mL-1 (OTA), 1.1 ng mL-1 (PAT), 7.9 ng mL-1 (HMF), and 1.0 ng mL-1 (BPA). Recoveries ranged from 82% to 99%. Good relative standard deviations for intraday retention times (≤3.54%) and peak area (≤3.5%) were achieved. The developed multi-contaminants analysis method was successfully applied to determine OTA, PAT, HMF, and BPA in various fruit drinks.

A Critical Review on Metal-Organic Frameworks and Their Composites as Advanced Materials for Adsorption and Photocatalytic Degradation of Emerging Organic Pollutants from Wastewater.

Water-borne emerging pollutants are among the greatest concern of our modern society. Many of these pollutants are categorized as endocrine disruptors due to their environmental toxicities. They are harmful to humans, aquatic animals, and plants, to the larger extent, destroying the ecosystem. Thus, effective environmental remediations of these pollutants became necessary. Among the various remediation techniques, adsorption and photocatalytic degradation have been single out as the most promising. This review is devoted to the compilations and analysis of the role of metal-organic frameworks (MOFs) and their composites as potential materials for such applications. Emerging organic pollutants, like dyes, herbicides, pesticides, pharmaceutical products, phenols, polycyclic aromatic hydrocarbons, and perfluorinated alkyl substances, have been extensively studied. Important parameters that affect these processes, such as surface area, bandgap, percentage removal, equilibrium time, adsorption capacity, and recyclability, are documented. Finally, we paint the current scenario and challenges that need to be addressed for MOFs and their composites to be exploited for commercial applications.