The aim of this study is to report the yield of extraction, as well as the physicochemical and antioxidant properties of extracted chitosan from mud crabs (S.olivacea) as compared to commercial chitosan. The yield obtained for extracted chitosan was 44.57 ± 3.44 % with a moisture and ash content of 9.48 ± 0.59 % and 5.97 ± 0.90 %, respectively. Commercial chitosan demonstrated a higher degree of deacetylation (58.42 ± 2.67 %), water (250 ± 9.90 %) and fat (329 ± 7.07 %) binding capacity, solubility (73.85 %), viscosity (463.25 ± 13.10 %) and also the whiteness value (77.8 ± 0.47) compared to the extracted chitosan, which were only 53.42 ± 0.88 %, 180 ± 0.00 %, 260 ± 0.00 %, 53.38 %, 383.9 ± 28.43 % and 62.1 ± 7.52 %, respectively. The structure of extracted and commercial chitosan was also investigated using Fourier Transform Infrared Spectroscopy (FTIR). In conclusion, the extracted chitosan possessed potential properties similar to the commercial chitosan with high reducing power but low in the scavenging activity on the DPPH and hydroxyl radicals compared to the commercial chitosan.
The issue of heavy metal contamination has caused a great deal of concern among water quality experts today, as it contributes to water pollution. Activated carbon nanofibers (ACNFs) showed a significant ability in removing heavy metals from the wastewater. In this study, polyacrylonitrile (PAN) was blended and electrospun with an abundant and inexpensive biopolymer, lignin and a water soluble polymer, poly(ethylene glycol) (PEG), by using an electrospinning technique to form nanofibers. The electrospun nanofibers were then investigated as a precursor for the production of porous ACNFs to study the removal of nickel(II) ions by adsorption technique. PEG was added to act as a porogen and to create the porous structure of carbon nanofibers (CNFs). CNFs were prepared by thermal treatment of the electrospun nanofibers and followed by activation of CNFs by thermal and acid treatment on CNFs. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) spectral analysis of the ACNFs showed a strong absorption peak of the C-O functional group, indicating the increase in the oxygenated compound. Field emission scanning electron microscopy (FESEM) images concluded that the ACNFs have more porous and compact fibers with a smaller fiber diameter of 263 ± 11 nm, while the CNFs are less compact and have slightly larger fiber diameter of 323 ± 6 nm. The adsorption study showed that the ACNFs possessed a much higher adsorption capacity of 18.09 mg/g compared with the CNFs, which the amount adsorbed was achieved only at 2.7 mg/g. The optimum adsorption conditions that gave the highest percentage of 60% for nickel(II) ions removal were 50 mg of adsorbent dosage, 100 ppm of nickel(II) solution, pH 3, and a contact time of 60 min. The study demonstrated that the fabrication of ACNFs from PAN/lignin/PEG electrospun nanofibers have potential as adsorbents for the removal of heavy metal contaminants.
Thirty milled rice samples were collected from retailers in 4 provinces of Malaysia. These samples were evaluated for Aspergillus spp. infection by direct plating on malt extract salt agar (MESA). All Aspergillus holomorphs were isolated and identified using nucleotide sequences of ITS 1 and ITS 2 of rDNA. Five anamorphs (Aspergillus flavus, A. oryzae, A. tamarii, A. fumigatus and A. niger) and 5 teleomorphs (Eurotium rubrum, E. amstelodami, E. chevalieri, E. cristatum and E. tonophilum) were identified. The PCR-sequencing based technique for sequences of ITS 1 and ITS 2 is a fast technique for identification of Aspergillus and Eurotium species, although it doesn't work flawlessly for differentiation of Eurotium species. All Aspergillus and Eurotium isolates were screened for their ability to produce aflatoxin and ochratoxin A (OTA) by HPLC and TLC techniques. Only A. flavus isolate UPM 89 was able to produce aflatoxins B1 and B2.
Symptoms of water-soaked lesions and soft rot were first observed in June 2011 on bell pepper fruits (Capsicum annuum cv. Annuum) in the two main regions of pepper production in Malaysia (Cameron Highlands and Johor State). Economic losses exceeded 40% in severely infected fields and greenhouses with the estimated disease incidence of 70%. In pepper fruits damaged by insects, sunscald, or other factors, symptoms initially appeared in the peduncle and calyx tissues and entire fruits were turned into watery masses within 2 to 6 days. Fruits infected in the field tended to collapse and hang on the plant. When the contents leaked out, the outer skin of the fruit dried and remained attached to the plant. Field-grown transplants and infected soil were identified as probable sources of inocula. A total of 50 attached fruits were collected from 10 pepper fields and greenhouses located in the two growing regions. Tissue from the margins of water-soaked lesions was surface-sterilized in 1% NaOCl for 2 min, rinsed in sterile water, dried, and plated onto nutrient agar (NA) and eosin methylene blue agar (EMB) media (3). A similar bacterium was isolated from all samples. After 2 days, white to creamy bacterial colonies on NA and emerald green colonies on EMB developed. Five independent strains were subjected to further biochemical, molecular, and pathogenicity tests. Bacterial strains were gram-negative, motile rods, grew at 37°C, were facultatively anaerobic, oxidase-negative, phosphatase-negative, and catalase-positive. They degraded pectate, were sensitive to erythromycin, did not utilize Keto-methyl glucoside, were indole production-negative, and reduced sugars from sucrose (3). Acid production was negative from sorbitol and arabitol, but positive from melibiose and citrate. PCR amplification of the pel gene by Y1 and Y2 primers produced a 434-bp fragment (2). Amplification of the intergenic transcribed spacer (ITS) region by G1 and L1 primers (4) gave two amplicons ca. 550 and 580 bp long. The expected amplicon was not produced with any of the strains using primers Br1f/L1r and Eca1f/Eca2r (1), whereas a 550-bp PCR product, typical of Pectobacterium carotovorum subsp. carotovorum, was obtained with primers EXPCCF and EXPCCR (1). Based on biochemical and molecular characteristics, and analysis of PCR-RFLP of 16S-ITS-23R rRNA genes using Rsa I enzyme (4), all five bacterial strains were identified as P. carotovorum subsp. carotovorum. BLAST analysis of the 16S rRNA sequence (GenBank Accession No KC189032) showed 100% identity to the 16S rRNA of P. carotovorum subsp. carotovorum strain PPC192. For pathogenicity tests, four mature pepper fruits of cv. Annuum were inoculated by injecting 10 μl of a bacterial suspension (108 CFU/ml) into pericarps and the fruits were incubated in a moist chamber at 80 to 90% relative humidity and 30°C. After 72 h, water-soaked lesions similar to those observed in the fields and greenhouses were observed and bacteria with the same characteristics were consistently reisolated, thereby fulfilling Koch's postulates. Symptoms were not observed on water-inoculated controls. References: (1) S. Baghaee-Ravari et al. Eur. J. Plant Pathol. 129:413, 2001. (2) A. Darraas et al. Appl. Environ. Microbiol. 60:1437, 1994. (3) N. W Schaad et al. Laboratory Guide for the Identification of Plant Pathogenic Bacteria. 3rd ed. The American Phytopathological Society Press, St Paul, MN, 2001. (4) I. K. Toth et al. Appl. Environ. Microbiol. 67:4070, 2001.
In August 2011, sweet potato (Ipomoea batatas), tomato (Solanum lycopersicum), and eggplant (S. melongena) crops from major growing areas of the Cameron highlands and Johor state in Malaysia were affected by a soft rot disease. Disease incidence exceeded 80, 75, and 65% in severely infected fields and greenhouses of sweet potato, tomato, and eggplant, respectively. The disease was characterized by dark and small water-soaked lesions or soft rot symptoms on sweet potato tubers, tomato stems, and eggplant fruits. In addition, extensive discoloration of vascular tissues, stem hollowness, and water-soaked, soft, dark green lesions that turned brown with age were observed on the stem of tomato and eggplant. A survey was performed in these growing areas and 22 isolates of the pathogen were obtained from sweet potato (12 isolates), tomato (6 isolates), and eggplant (4 isolates) on nutrient agar (NA) and eosin methylene blue (EMB) (4). The cultures were incubated at 27°C for 2 days and colonies that were emerald green on EMB or white to gray on NA were selected for further studies. All bacterial cultures isolated from the survey exhibited pectolytic ability on potato slices. These bacterial isolates were gram negative; rod shaped; N-acetylglucosaminyl transferase, gelatin liquefaction, and OPNG positive; and were also positive for acid production from D-galactose, lactosemelibiose, raffinose, citrate, and trehalose. They were negative for indol production, phosphatase activity, reducing substances from sucrose, and negative for acid production from maltose, sorbitol, inositol, inolin, melezitose, α-mathyl-D-glocoside, and D-arabitol. The bacteria did not grow on NA at 37°C. Based on these biochemical and morphological assays, the pathogen was identified as Pectobacterium wasabiae (2). In addition, DNA was extracted and PCR assay with two primers (16SF1 and 16SR1) was performed (4). Partial sequences of 16S rRNA (GenBank Accession Nos. JQ665714, JX494234, and JX513960) of sweet potato, tomato, and eggplant, respectively, exhibited a 99% identity with P. wasabiae strain SR91 (NR_026047 and NR_026047.1). A pathogenicity assay was carried out on sweet potato tubers (cv. Oren), tomato stems (cv. 152177-A), and eggplant fruits (cv. 125066x) with 4 randomly representative isolates obtained from each crop. Sweet potato tubers, tomato stems, and eggplant fruits (4 replications) were sanitized in 70% ethyl alcohol for 30 s, washed and rinsed in sterile distilled water, and needle punctured with a bacterial suspension at a concentration of 108 CFU/ml. Inoculated tubers, stems, and fruits were incubated in a moist chamber at 90 to 100% RH for 72 h at 25°C when lesions were measured. All inoculated tubers, stems, and fruits exhibited soft rot symptoms after 72 h similar to those observed in the fields and greenhouses and the same bacteria were consistently reisolated. Symptoms were not observed on controls. The pathogenicty test was repeated with similar results. P. wasabiae have been previously reported to cause soft rot on Japanese horseradish (3), and aerial stem rot on potato in New Zealand (4), the U.S. (2), and Iran (1). To our knowledge, this is the first report of sweet potato, tomato, and eggplant soft rot caused by P. wasabiae in Malaysia. References: (1) S. Baghaee-Ravari et al. Eur. J. Plant Pathol. 129:413, 2011. (2) S. De Boer and A. Kelman. Page 56 in: Laboratory Guide for Identification of Plant Pathogenic Bacteria, 3rd ed. N. Schaad et al., eds. APS Press, St. Paul, 2001. (3) M. Goto et al. Int. J. Syst. Bacteriol. 37:130, 1987. (4) A. R. Pitman et al. Eur. J. Plant Pathol. 126:423, 2010.
BACKGROUND: Some routes of transmission of Escherichia coli O157:H7 to fresh produce include contaminated irrigation water and manure polluted soils. The aim of the present study was to determine the genetic relationships of E. coli O157:H7 isolated from some produce growing region in Nigeria using enterobacterial repetitive intergenic consensus (ERIC) DNA fingerprinting analysis. A total of 440 samples comprising leafy greens, irrigation water, manure and soil were obtained from vegetable producing regions in Kano and Plateau States, Nigeria. Genes coding for the quinolone resistance-determinant (gyrA) and plasmid (pCT) coding for multidrug resistance (MDR) were determined using polymerase chain reaction (PCR) in 16 isolates that showed MDR.
RESULTS: Cluster analysis of the ERIC-PCR profiles based on band sizes revealed six main clusters from the sixteen isolates analysed. The largest cluster (cluster 3) grouped isolates from vegetables and manure at a similarity coefficient of 0.72.
A nanocomposite consisting of electrochemically reduced graphene oxide, poly(Eriochrome black T) and gold nanoparticles (ERGO-pEBT/AuNPs) was prepared for the simultaneous detection of resorcinol (RC), catechol (CC), and hydroquinone (HQ). The electrochemical oxidation of HQ, CC, and RC was analysed by using cyclic voltammetry and differential pulse voltammetry. Three well-separated potentials were found at 166, 277, and 660 mV (vs. Ag/AgCl) for HQ, CC, and RC, respectively The linear ranges were 0.52-31.4, 1.44-31.2, and 3.8-72.2 μM for HQ, CC, and RC, respectively. The limits of detections (LODs) for both individual and simultaneous detections are negligibly different are (15, 8, and 39 nM, respectively). Graphical abstract Voltammetric determination of hydroquinone, catechol, and resorcinol at ERGO-pEBT/AuNPs resulted in high peak currents and outstanding oxidation potential separation of the analytes.
Water pollution issues, particularly those caused by heavy metal ions, have been significantly growing. This paper combined biopolymers such as sodium alginate (SA) and β-cyclodextrin (β-CD) to improve adsorption performance with the help of calcium ion as the cross-linked agent. Moreover, the addition of carbon nanotubes (CNTs) into the hybrid hydrogel matrix was examined. The adsorption of nickel(II) was thoroughly compared between pristine sodium alginate/β-cyclodextrin (SA-β-CD) and sodium alginate/β-cyclodextrin immobilized carbon nanotubes (SA-β-CD/CNTs) hydrogel. Both hydrogels were characterized by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) spectral analysis, field emission scanning electron microscopy (FESEM), electron dispersive spectroscopy (EDX), thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) surface area analysis. The results showed SA-β-CD/CNTs hydrogel exhibits excellent thermal stability, high specific surface area and large porosity compared with SA-β-CD hydrogel. Batch experiments were performed to study the effect of several adsorptive variables such as initial concentration, pH, contact time and temperature. The adsorption performance of the prepared SA-β-CD/CNTs hydrogel was comprehensively reported with maximum percentage removal of up to 79.86% for SA-β-CD/CNTs and 69.54% for SA-β-CD. The optimum adsorption conditions were reported when the concentration of Ni(II) solution was maintained at 100 ppm, pH 5, 303 K, and contacted for 120 min with a 1000 mg dosage. The Freundlich isotherm and pseudo-second order kinetic model are the best fits to describe the adsorption behavior. A thermodynamic study was also performed. The probable interaction mechanisms that enable the successful binding of Ni(II) on hydrogels, including electrostatic attraction, ion exchange, surface complexation, coordination binding and host-guest interaction between the cationic sites of Ni(II) on both SA-β-CD and SA-β-CD/CNTs hydrogel during the adsorption process, were discussed. The regeneration study also revealed the high efficiency of SA-β-CD/CNTs hydrogel on four successive cycles compared with SA-β-CD hydrogel. Therefore, this work signifies SA-β-CD/CNTs hydrogel has great potential to remove Ni(II) from an aqueous environment compared with SA-β-CD hydrogel.
A simple adsorption/desorption procedure using a mixed matrix membrane (MMM) as extraction medium is demonstrated as a new miniaturized sample pretreatment and preconcentration technique. Reversed-phase particles namely polymeric bonded octadecyl (C18) was incorporated through dispersion in a cellulose triacetate (CTA) polymer matrix to form a C18-MMM. Non-steroidal anti-inflammatory drugs (NSAIDs) namely diclofenac, mefenamic acid and ibuprofen present in the environmental water samples were selected as targeted model analytes. The extraction setup is simple by dipping a small piece of C18-MMM (7 mm × 7 mm) in a stirred 10 mL sample solution for analyte adsorption process. The entrapped analyte within the membrane was then desorbed into 100 μL of methanol by ultrasonication prior to high performance liquid chromatography (HPLC) analysis. Each membrane was discarded after single use to avoid any analyte carry-over effect. Several important parameters, such as effect of sample pH, salting-out effect, sample volume, extraction time, desorption solvent and desorption time were comprehensively optimized. The C18-MMM demonstrated high affinity for NSAIDs spiked in tap and river water with relative recoveries ranging from 92 to 100% and good reproducibility with relative standard deviations between 1.1 and 5.5% (n=9). The overall results obtained were found comparable against conventional solid phase extraction (SPE) using cartridge packed with identical C18 adsorbent.
The present study deals with the synthesis, characterization, and DNA extraction of poly(4,4'-cyclohexylidene bisphenol oxalate)/silica (Si) nanocomposites (NCs). The effects of varying the monomer/Si (3.7%, 7%, and 13%) ratio towards the size and morphology of the resulting NC and its DNA extraction capabilities have also been studied. For the NC synthesis, two different methods were followed, including the direct mixing of poly(4,4'-cyclohexylidene bisphenol oxalate) with fumed Si, and in situ polymerization of the 4,4'-cyclohexylidene bisphenol monomer in the presence of fumed silica (11 nm). The formed NCs were thoroughly investigated by using different techniques such as scanning electron microscopy (SEM), fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), powdered X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) analysis where the results supported that there was the successful formation of poly(4,4'-cyclohexylidene bisphenol oxalate)/Si NC. Within the three different NC samples, the one with 13% Si was found to maintain a very high surface area of 12.237 m²/g, as compared to the other two samples consisting of 7% Si (3.362 m²/g) and 3.7% Si (1.788 m²/g). Further, the solid phase DNA extraction studies indicated that the efficiency is strongly influenced by the amount of polymer (0.2 g > 0.1 g > 0.02 g) and the type of binding buffer. Among the three binding buffers tested, the guanidine hydrochloride/EtOH buffer produced the most satisfactory results in terms of yield (1,348,000 ng) and extraction efficiency (3370 ng/mL) as compared to the other two buffers of NaCl (2 M) and phosphate buffered silane. Based on our results, it can be indicated that the developed poly(4,4'-cyclohexylidene bisphenol oxalate)/Si NC can serve as one of the suitable candidates for the extraction of DNA in high amounts as compared to other traditional solid phase approaches.
A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile-0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1-10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3-114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis.
This study describes a dispersive liquid-liquid microextraction combined with dispersive solid-phase extraction method based on phenyl-functionalized magnetic sorbent for the preconcentration of polycyclic aromatic hydrocarbons from environmental water, sugarcane juice, and tea samples prior to gas chromatography with mass spectrometry analysis. Several important parameters affecting the extraction efficiency were investigated thoroughly, including the mass of sorbent, type and volume of extraction solvent, extraction time, type of desorption solvent, desorption time, type and amount of salt-induced demulsifier, and sample volume. Under the optimized extraction and gas chromatography-mass spectrometric conditions, the method revealed good linearity (10-100000 ng/L) with coefficient of determination (R2 ) of ≥0.9951, low limits of detection (3-16 ng/L), high enrichment factors (61-239), and satisfactory analyte recoveries (86.3-109.1%) with the relative standard deviations
Superhydrophilic graphene oxide/electrospun cellulose nanofibre (GO/CNF) was synthesized, characterized and successfully used in a solid-phase membrane tip adsorption (SPMTA) as an adsorbent towards a simultaneous analysis of polar organophosphorus pesticides (OPPs) in several food and water samples. Separation, determination and quantification were achieved prior to ultra-performance liquid chromatography coupled with ultraviolet detector. The influence of several parameters such as sample pH, adsorption time, adsorbent dosage and initial concentration were investigated. SPMTA was linear in the range of 0.05 and 10 mg l-1 under the optimum adsorption conditions (sample pH 12; 5 mg of adsorbent dosage; 15 min of adsorption time) for methyl parathion, ethoprophos, sulfotepp and chlorpyrifos with excellent correlation coefficients of 0.994-0.999. Acceptable precision (RSDs) as achieved for intraday (0.06-5.44%, n = 3) and interday (0.17-7.76%, n = 3) analyses. Low limits of detection (0.01-0.05 mg l-1) and satisfactory consistency in adsorption (71.14-99.95%) were obtained for the spiked OPPs from Sungai Pahang, Tasik Cheras, cabbages and rice samples. The adsorption data were well followed the second-order kinetic model and fits the Freundlich adsorption model. The newly synthesized GO/CNF showed a great adsorbent potential for OPPs analysis.
Molecularly imprinted polymers (MIPs) are synthetic polymers with a predetermined selectivity for a particular analyte or group of structurally related compounds, making them ideal materials for separation processes. Hence, in sample preparation, MIPs are chosen as an excellent material to provide selectivity. Moreover, its use in solid-phase extraction, also referred to as molecular imprinted solid phase extraction (MISPE), is well regarded. In recent years, many papers have been published addressing the utilization of MIPs or MISPE as sorbents in natural product applications, such as synthesis. This review describes the synthesis and characterization of MIPs as a tool in natural product applications.
A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r2 = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of <8.0% (n = 5) for the determination of 0.1, 5.0, and 500.0 μg/L of antidepressant drugs. This method was successfully applied to the determination of amitriptyline and chlorpromazine in plasma and urine samples. The recoveries of spiked plasma and urine samples were in the range of 86.1-115.4%. Results indicate that magnetite micro-solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples.
In the present study, iminodiacetic acid (IDA)-modified kenaf fiber, K-IDA formed by the chemical modification of plant kenaf biomass was tested for its efficacy as a sorbent material towards the purification of waste water. The K-IDA fiber was first characterized by the instrumental techniques like Fourier transform infrared (FTIR) analysis, elemental analysis (CHNSO), and scanning electron microscopy (SEM). On testing for the biosorption, we found that the K-IDA has an increment in the adsorption of Cu2+ ions as compared against the untreated fiber. The Cu2+ ions adsorption onto K-IDA fits very well with the Langmuir model and the adsorption maximum achieved to be 91.74mg/g. Further, the adsorption kinetics observed to be pseudo second-order kinetics model and the Cu2+ ions adsorption is a spontaneous endothermic process. The desorption study indicates a highest percentage of Cu2+ of 97.59% from K-IDA under 1M HCl solution against H2SO4 (72.59%) and HNO3 (68.66%). The reusability study indicates that the efficiency did not change much until the 4th cycle and also providing enough evidence for the engagement of our biodegradable K-IDA fiber towards the removal of Cu2+ ions in real-time waste water samples obtained from the electroplating and wood treatment industries.
Molecularly imprinted polymer (MIP) was employed as sorbent in ultrasound assisted emulsification molecularly imprinted polymer micro-solid phase extraction (USAE-MIP-µ-SPE) of bisphenol A (BPA) in water, beverages and the aqueous liquid in canned foods prior to high performance liquid chromatography-diode array detector (HPLC-DAD) analysis. Several effective variables, such as types of emulsification solvent and its volume, types of desorption solvent and its volume, salting out effect, pH of sample solution, mass of sorbent, extraction and desorption time, and sample volume, were optimized comprehensively. Under the optimized USAE-MIP-µ-SPE and HPLC-DAD conditions, the method demonstrated good linearity over the range of 0.5-700μgL-1with a coefficient determination of R2=0.9973, low limit of detection (0.07μgL-1), good analyte recoveries (82.2-118.9%) and acceptable RSDs (0.7-14.2%, n=3) with enrichment factor of 49. The method was applied to thirty samples of drinking water, mineral water, river water, lake water, as well as beverages and canned foods, the presence of BPA was identified in four samples. The proposed method showed good selectivity and reusability for extraction of BPA, and hence the USAE-MIP-µ-SPE is rapid, simple, cost effective and environmentally friendly.
We describe the preparation, characterization, and application of a composite film adsorbent based on blended agarose-chitosan-multiwalled carbon nanotubes for the preconcentration of selected nonsteroidal anti-inflammatory drugs in aqueous samples before determination by high performance liquid chromatography with ultraviolet detection. The composite film showed a high surface area (4.0258 m2 /g) and strong hydrogen bonding between the multiwalled carbon nanotubes and agarose/chitosan matrix, which prevent adsorbent deactivation and ensure long-term stability. Several parameters, such as sample pH, addition of salt, extraction time, desorption solvent, and concentration of multiwalled carbon nanotubes in the composite film were optimized using a one-factor-at-time approach. The optimum extraction conditions obtained were as follows: isopropanol as conditioning solvent, 10 mL of sample solution at pH 2, extraction time of 30 min, stirring speed of 600 rpm, 100 μL of isopropanol as desorption solvent, desorption time of 5 min under ultrasonication, and 0.4% w/v of composite film. Under the optimized conditions, the calibration curve showed good linearity in the range of 1-500 ng/mL (r2 = 0.997-0.999), and good limits of detection (0.89-8.05 ng/mL) were obtained with good relative standard deviations of
Recently, pharmaceutical pollutants in water have emerged as a global concern as they give threat to human health and the environment. In this study, graphene nanoplatelets (GNPs) were used to efficiently remove antibiotics sulfamethoxazole (SMX) and analgesic acetaminophen (ACM) as pharmaceutical pollutants from water by an adsorption process. GNPs; C750, C300, M15 and M5 were characterized by high-resolution transmission electron microscopy, Raman spectroscopy, X-ray diffraction and Brunauer-Emmett-Teller. The effects of several parameters viz. solution pH, adsorbent amount, initial concentration and contact time were studied. The parameters were optimized by a batch adsorption process and the maximum removal efficiency for both pharmaceuticals was 99%. The adsorption kinetics and isotherms models were employed, and the experimental data were best analysed with pseudo-second kinetic and Langmuir isotherm with maximum adsorption capacity (Qm) of 210.08 mg g-1 for SMX and 56.21 mg g-1 for ACM. A regeneration study was applied using different eluents; 5% ethanol-deionized water 0.005 M NaOH and HCl. GNP C300 was able to remove most of both pollutants from environmental water samples. Molecular docking was used to simulate the adsorption mechanism of GNP C300 towards SMX and ACM with a free binding energy of -7.54 kcal mol-1 and -5.29 kcal mol-1, respectively, which revealed adsorption occurred spontaneously.
Mesoporous silica material, MCM-41, was utilized for the first time as an adsorbent in solid phase membrane tip extraction (SPMTE) of non-steroidal anti-inflammatory drugs (NSAIDs) in urine prior to high performance liquid chromatography-ultraviolet (HPLC-UV) analysis. The prepared MCM-41 material was enclosed in a polypropylene membrane tip and used as an adsorbent in SPMTE. Four NSAIDs namely ketoprofen, diclofenac, mefenamic acid and naproxen were selected as model analytes. Several important parameters, such as conditioning solvent, sample pH, salting-out effect, sample volume, extraction time, desorption solvent and desorption time were optimized. Under the optimum extraction conditions, the MCM-41-SPMTE method showed good linearity in the range of 0.01-10μg/mL with excellent correlation coefficients (r=0.9977-0.9995), acceptable RSDs (0.4-9.4%, n=3), good limits of detection (5.7-10.6μg/L) and relative recoveries (81.4-108.1%). The developed method showed a good tolerance to biological sample matrices.