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.

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.

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.

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.

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.

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.

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.

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.

Salting-out assisted liquid-liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples.

In this study, salting-out assisted liquid-liquid extraction (SALLE) as a simple and efficient extraction technique followed by high-performance liquid chromatography (HPLC) was employed for the determination of vitamin D3 in milk samples. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. Under the optimum conditions, acetonitrile and ammonium sulfate were used as the extraction solvent and salting-out agent, respectively. The vitamin D3 extract was separated using Hypersil ODS (250x i.d 4.6 mm, 5 µm) HPLC column that was coupled with diode array detector. Vitamin D2 was used as internal standard (IS) to offset any variations in chromatographic conditions. The vitamin D3 and the IS were eluted in 18 min. Good linearity (r 2 > 0.99) was obtained within the range of 25-600 ng g-1 with the limit of detection of 15 ng g-1 and limit of quantification of 25 ng g-1. The validated method was applied for the determination of vitamin D3 in milk samples. The recoveries for spiked samples were from 94.4 to 113.5%.

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.

Molecularly imprinted silica gel incorporated with agarose polymer matrix as mixed matrix membrane for separation and preconcentration of sulfonamide antibiotics in water samples.

Molecularly imprinted silica gel (MISG) was incorporated through dispersion in agarose polymer matrix to form a mixed matrix membrane (MMM) and was applied for the determination of three sulfonamide antibiotic compounds (i.e. sulfamethoxazole (SMX), sulfamonomethoxine (SMM), and sulfadiazine (SDZ)) from environmental water samples. Several important microextraction conditions, such as type of desorption solvent, extraction time, amount of sorbent, sample volume, pH, and effect of desorption time, were comprehensively optimized. A preconcentration factors of ≥ 20 was achieved by the extraction of 12.5 mL of water samples using the developed method. This microextraction-HPLC method demonstrated good linearity (1-500 µg L-1) with a coefficient of determination (R2) of 0.9959-0.9999, low limits of detection (0.06-0.17 µg L-1) and limits of quantification (0.20-0.56 µg L-1), good analyte recoveries (80-96%), and acceptable relative standard deviations (< 10%) under the optimized conditions. The method is systematically compared to those reported in the literature.

Removal of anthracene in water by MIL-88(Fe), NH2-MIL-88(Fe), and mixed-MIL-88(Fe) metal-organic frameworks.

Three adsorbents based on the metal-organic frameworks (MOFs), viz.; MIL-88(Fe), NH2-MIL-88(Fe), and mixed-MIL-88(Fe) were synthesized using a microwave-assisted solvothermal technique. The as-synthesized MOFs were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), field emission scanning microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). The MOFs were shown to possess highly crystalline and porous structures with specific surface areas of 1240, 941, and 1025 m2 g-1 and pore volumes of 0.7, 0.6 and 0.6 m3 g-1 for MIL-88(Fe), NH2-MIL-88(Fe) and mixed-MIL-88(Fe), respectively. Faster removal of a model polycyclic aromatic hydrocarbon, anthracene (ANT) within 25 minutes, was achieved when these MOFs were used as adsorbents in water. The removal efficiency was 98.3, 92.4 and 95.8% for MIL-88(Fe), NH2-MIL-88(Fe) and mixed-MIL-88(Fe), respectively. The kinetics and isotherms of the process were best statistically described by pseudo-second-order and Langmuir models, respectively, while the thermodynamic studies revealed the exothermic and spontaneous nature of the process. Docking simulations were found to be consistent with the experimental results with MIL-88(Fe) showing the best binding capacity with the ANT molecule.

Thiol-functionalized magnetic carbon nanotubes for magnetic micro-solid phase extraction of sulfonamide antibiotics from milks and commercial chicken meat products.

Thiol-functionalized magnetic carbon nanotubes (TMCNTs) were employed as the sorbent in the magnetic micro-solid phase extraction (M-µ-SPE) of sulfonamide antibiotics (SAs) in water, milks and chicken meat products prior to high performance liquid chromatography-diode array detector (HPLC-DAD) analysis. The synthesized sorbent was characterized by several spectroscopic techniques. Optimum conditions were: 20 mg of TMCNTs at pH 4, 2 min extraction time, 10% addition of salt and 30 mL of sample volume. Under the optimized TMCNTs-M-µ-SPE and HPLC-DAD conditions, the method showed good linearity in the range of 0.1-500 µg L-1 (r2 ≥ 0.9950), low limits of detection (0.02-1.5 µg L-1), good analytes recovery (80.7-116.2%) and acceptable RSDs (0.3-7.7%, n = 15). The method was applied to tap water (1), milks (15) and commercial chicken meat products (35), SAs were detected in five chicken meat samples (3.0-25.7 µg L-1). The method is critically compared to those reported in the literature.

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.

Cyclodextrin based polymer sorbents for micro-solid phase extraction followed by liquid chromatography tandem mass spectrometry in determination of endogenous steroids.

Sorbents were prepared by cross-linking ß-cyclodextrin (ß-CD) using two different types of cross-linker units at variable reactant mole ratios. The resulting polymers containing ß-CD were evaluated as sorbents in micro-solid phase extraction (µ-SPE) format for the extraction of the endogenous steroids testosterone (T), epitestosterone (E), androsterone (A), etiocholanolone (Etio), 5α-androstane-3α,17ß-diol (5αAdiol) and 5ß-androstane-3α,17ß-diol (5ßAdiol). The best sorbent (C1; cyclodextrin polymer) showed superior extraction characteristics compared with commercial sorbents (C18 and Bond Elut Plexa). Parameters influencing the extraction efficiency of the C1 sorbent such as extraction and desorption times, desorption solvent and volume of sample were investigated. The extracts were separated using a Hypersil Gold column (50 × 2.1 mm, 1.9 µm) under gradient elution coupled to a LC-MS/MS. The compounds were successfully separated within 8 min. The method offers good repeatability (RSD < 10%) and linearity (r2 > 0.995) were within the range of 1-200 ng mL-1 for T and E, 250-4000 ng mL-1 for A and Etio and 25-500 ng mL-1 for 5αAdiol and 5ßAdiol, respectively. The method was applied for the determination of steroid profile of urine from volunteers.

Salting-out assisted liquid-liquid extraction coupled with hydrophilic interaction chromatography for the determination of biguanides in biological and environmental samples.

A new salting-out assisted liquid-liquid extraction (SALLE) sample preparation method for the determination of the polar anti-diabetic biguanide drugs (metformin, buformin and phenformin) in blood plasma, urine and lake water samples were developed. The SALLE was performed by mixing samples (plasma (0.2mL), urine or lake water (1.0mL)) with acetonitrile (0.4mL for plasma, 0.5mL for urine or lake water), sodium hydroxide powder was then added for the phase separation. The effects of type of salting-out reagent, type of extraction solvent, volumes of acetonitrile and sample, amount of sodium hydroxide, vortexing and centrifugation times on the extraction efficiency were investigated. The upper layer, containing the biguanides, was directly injected into a HPLC unit using ZIC-HILIC column (150mm×2.1mm×3.5µm) and was detected at 236nm. The method was validated and calibration curves were linear with r2>0.99 over the range of 20-2000µgL-1 for plasma and 5-2000µgL-1 for urine and lake water samples. The limits of detection were in the range (3.8-5.6)µgL-1, (0.8-1.5)µgL-1 and (0.3-0.8)µgL-1 for plasma, urine and lake water, respectively. The accuracies in the three matrices were within 87.3-103%, 87.4-109%, 82.2-109% of the nominal concentration for metformin, buformin and phenformin, respectively. The relative standard deviation for inter- and intra -day precision were in the range of 1.0-17% for all analytes in the three matrices.

Liquid Chromatographic Analysis of α-Dicarbonyls Using Girard-T Reagent Derivatives.

The measurement of α-dicarbonyls and other degradation products of sugars has become important in view of their toxicity. Although there are several methods used for their analysis, most require long reaction times to form UV absorbing or fluorescent derivatives and the nonpolar nature of commonly used derivatives necessitates relatively high concentrations of organic solvents for elution in reverse phase liquid chromatography. The present method describes the use of Girard-T reagent in a simple, one step derivatization of α-dicarbonyls and conjugated aldehydes and analysis using ion-pair reverse phase liquid chromatography. The limit of detection was in the range of 0.06-0.09 µM (4-12 ng/mL) for glyoxal, methylglyoxal, 3-deoxyglucosone and 5-hydroxymethylfurfural with good linear response and reproducibility using UV detection. The hydrazone derivatives were stable for several days in solution. The method was used to study degradation of several sugars and quantification of the target α-dicarbonyls and 5-hydroxymethylfurfural in several soft drinks.

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.