Electrochemical enzyme-based blood uric acid biosensor: new insight into the enzyme immobilization on the surface of electrode via poly-histidine tag.

In a new approach, we considered the special affinity between Ni and poly-histidine tags of recombinant urate oxidase to utilize Ni-MOF for immobilizing the enzyme. In this study, a carbon paste electrode (CPE) was modified by histidine-tailed urate oxidase (H-UOX) and nickel-metal-organic framework (Ni-MOF) to construct H-UOX/Ni-MOF/CPE, which is a rapid, sensitive, and simple electrochemical biosensor for UA detection. The use of carboxy-terminal histidine-tailed urate oxidase in the construction of the electrode allows the urate oxidase enzyme to be positioned correctly in the electrode. This, in turn, enhances the efficiency of the biosensor. Characterization was carried out by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET), and field emission scanning electron microscopy (FE-SEM). At optimum conditions, the biosensor provided a short response time, linear response within 0.3-10 µM and 10-140 µM for UA with a detection limit of 0.084 µM, repeatability of 3.06%, and reproducibility of 4.9%. Furthermore, the biosensor revealed acceptable stability and selectivity of UA detection in the presence of the commonly coexisted ascorbic acid, dopamine, L-cysteine, urea, and glucose. The detection potential was at 0.4 V vs. Ag/AgCl.

Epidemiology of Asthma in Patients with COVID-19: Investigation of Respiratory Allergy as a Risk Factor for COVID-19 Severity.

Background: The outcome of coronavirus disease 2019 (COVID-19) is complicated by various comorbidities; asthma, a common chronic disease, may be considered one of these conditions. This study aimed to investigate the effect of asthma as a potential comorbid condition on the COVID-19 prognosis. Materials and Methods: This retrospective study included all RT-PCR confirmed COVID-19 cases recorded on the Shiraz health department's electronic database from January to May 2020. A questionnaire was designed to collect information about patients' demographics, their history of asthma and other comorbidities, and the severity of COVID-19 by contacting them by phone. Results: Of 3163 COVID-19 patients, 109 (3.4%) had self-reported asthma with a mean age of 42.7 ± 19.1 years. Most patients (98%) had mild-to-moderate asthma, while 2% had severe disease. Among asthmatic patients, fourteen (12.8%) were admitted to the hospital, and five (4.6%) died. Univariate logistic regression results showed that asthma had no significant effect on hospitalization (OR 0.95, 95% CI: 0.54-1.63) and mortality (OR 1.18, 95% CI: 0.48-2.94) in patients with COVID-19. Compared living and deceased patients with COVID-19, the pooled OR was 18.2 (95% CI: 7.3-40.1) for cancer, 13.5 (95% CI: 8.2-22.5) for age 40-70 years, 3.1 (95% CI: 2-4.8) for hypertension, 3.1 (95% CI: 1.8-5.3) for cardiac disease and 2.1 (95% CI: 1.3-3.5) for diabetes mellitus. Conclusion: This study showed that asthma is not associated with an increased risk of hospitalization and mortality in patients with COVID-19. Further studies are needed to investigate the risk of different asthma phenotypes on the severity of COVID-19 disease.

Developing a novel sensor based on ionic liquid molecularly imprinted polymer/gold nanoparticles/graphene oxide for the selective determination of an anti-cancer drug imiquimod.

Despite its useful properties, imiquimod (IMQ), known as an anti-cancer drug, can be harmful to the skin at high concentrations. Therefore, we have developed a novel electrochemical sensor to determine IMQ, for the first time. A glassy carbon electrode (GCE) was modified by a new composite comprising of ionic liquid-based molecularly imprinted polymer (MIP) and gold nanoparticles/graphene oxide (Au/GO). The MIP/Au/GO nanocomposite was synthesized through non-covalent imprinting process in the presence of IMQ, as template molecule and characterized by SEM and FT-IR. The square wave voltammetry technique (SWV) was applied for IMQ determination in 0.1 M phosphate buffer solution (PBS) at pH 7.0. Several parameters affecting the IMQ quantification were evaluated and optimized. Under the optimized conditions, the sensor presented a linear range of 0.02-20.0 µM, a limit of quantification and detection of 0.02 µM and 0.006 µM, respectively. Low RSD values indicate the good repeatability and reproducibility of the modified electrodes in preparation and determination procedures. The satisfactory results indicated that the proposed sensor could be successfully applied for IMQ determination in real samples.

The anticonvulsant effects of Ducrosia anethifolia (Boiss) essential oil are produced by its main component alpha-pinene in rats.

BACKGROUND: Ducrosia anethifolia has been recommended as a remedy for neurological disorders. However, the anticonvulsant effects of D. anethifolia essential oil (DAEO) and its major constituent α-pinene have not yet been clarified. METHODS: A rat model of pentylenetetrazole (PTZ)-induced convulsions was used. Oxidant and antioxidant parameters were assayed in the temporal lobe. RESULTS: The data showed that DAEO (50, 100 and 200 mg/kg, i.p.) and α-pinene (0.2 and 0.4 mg/kg i.p.) delayed the initiation time, and reduced the duration of myoclonic and tonic-clonic seizures following PTZ injection. The PTZ produced oxidative stress so that malondialdehyde and hydrogen peroxide levels were increased and catalase and peroxidase activity decreased. Pretreatment with DAEO and α-pinene significantly inhibited the above-mentioned enzymatic changes in PTZ-treated animals. CONCLUSION: The results suggest that α-pinene, at teast in part, was responsible for the induction of the anticonvulsant and antioxidant effects of DAEO in rats.

The anticonvulsant effects of Ducrosia anethifolia (Boiss) essential oil are produced by its main component alpha-pinene in rats / Os efeitos anticonvulsivantes do óleo essencial de Ducrosia anethifolia (Boiss) são realizados pelo seu principal componente alfa-pineno em ratos

ABSTRACT Ducrosia anethifolia has been recommended as a remedy for neurological disorders. However, the anticonvulsant effects of D. anethifolia essential oil (DAEO) and its major constituent α-pinene have not yet been clarified. Methods: A rat model of pentylenetetrazole (PTZ)-induced convulsions was used. Oxidant and antioxidant parameters were assayed in the temporal lobe. Results: The data showed that DAEO (50, 100 and 200 mg/kg, i.p.) and α-pinene (0.2 and 0.4 mg/kg i.p.) delayed the initiation time, and reduced the duration of myoclonic and tonic-clonic seizures following PTZ injection. The PTZ produced oxidative stress so that malondialdehyde and hydrogen peroxide levels were increased and catalase and peroxidase activity decreased. Pretreatment with DAEO and α-pinene significantly inhibited the above-mentioned enzymatic changes in PTZ-treated animals. Conclusion: The results suggest that α-pinene, at teast in part, was responsible for the induction of the anticonvulsant and antioxidant effects of DAEO in rats.

RESUMO A Ducrosia anethifolia tem sido recomendada como remédio para os distúrbios neurológicos. No entanto, os efeitos anticonvulsivantes do óleo essencial de Ducrosia anethifolia (DAEO) e do seu principal constituinte atfa-pineno (α-pineno) ainda não foram clarificados. Métodos: Foi utilizado um modelo de rato de convulsões induzidas por pentilenotetrazol (PTZ). Os parâmetros oxidante e antioxidante foram ensaiados no lobo temporal do cérebro. Resultados: Os dados mostraram que DAEO (50, 100 e 200 mg / kg, i.p.) e α-pineno (0,2 e 0,4 mg / kg i.p.) retardaram o tempo de iniciação e reduziram a duração das crises mioclônicas e tônico-clônicas após a injeção de PTZ. O PTZ produziu estresse oxidativo, de modo que os níveis de malondialdeído (MDA) e de peróxido de hidrogênio aumentaram e a atividade da catalase e da peroxidase diminuiu. O pré-tratamento com DAEO e α-pineno inibiu significativamente as alterações enzimáticas mencionadas em animais tratados com PTZ. Conclusão: O resultado sugere que α-pineno, peto menos em parte, é responsável peta indução dos efeitos anticonvulsivantes e antioxidantes da DAEO em ratos.

Decoration of graphene oxide with NiO@polypyrrole core-shell nanoparticles for the sensitive and selective electrochemical determination of piceatannol in grape skin and urine samples.

For the first time, we developed an electrochemical sensor for piceatannol based on a new type of nanocomposite: graphene oxide nano sheets decorated with core-shell NiO@polypyrrole nanoparticles (NiO@Ppy/GO) mixed with nafion and casted on the surface of glassy carbon electrode. The nanocomposite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction and Fourier transform infrared spectroscopy (FT-IR) techniques. The square wave voltammetry as a sensitive technique and cyclic voltammetry were selected for the quantification of piceatannol in 0.1 M phosphate buffer solution (pH 7.0). Several parameters were evaluated such as pH value, scan rate and supporting electrolyte type for the determination of piceatannol. In addition, selectivity and repeatability measurements were also evaluated. Under the optimized conditions, linear range and limit of detection were obtained 0.01-10.0 µM and 0.003 µM, respectively. Relative standard deviation for 3.0 µM and 6.5 µM were calculated 3.25% and 1.83%, respectively. The proposed sensor was applied successfully for the quantification analysis of piceatannol in grape skin essential oil and urine sample with satisfactory results.

Effects of oregano essential oil on brain TLR4 and TLR2 gene expression and depressive-like behavior in a rat model.

The aim of the present study was to evaluate the effects of oregano essential oil (OEO) on the hippocampus and prefrontal cortex TLR 2/4 gene expression and depressive like behavior induced by chronic unpredictable stress (CUS). Sucrose preference and forced swim tests were adopted to examine the antidepressant effect. Control (CON), OEO, CUS, and CUS + OEO groups were used. The OEO and CUS + OEO groups received OEO (0.2 mL/kg, i.p.), CON and CUS received saline (0.2 mL/kg, i.p.), and the positive drug groups of CUS rats received fluoxetine (10 mg/kg) and diazepam (3 mg/kg) once daily for 14 days. The expression of TLR 2/4 was determined using real time quantitative polymerase chain reaction with the SYBR green reporter dye. The compositions of the OEO were determined by gas chromatography-mass spectroscopy. The main constituents were thymol (20.72%), gamma-terpinene (8.83%), borneol (8.72%), cymene (6.83%), carvacrol (6.274%), alfa-terpinene (5.26%), and sabinene (4.92%). Administration of OEO significantly alleviated the depressive symptoms of CUS. A higher level of TLR2/4 mRNA was seen in the brain of CUS group (P < 0.05). The CUS-induced increases in the TLR2/4 levels were not reversed by OEO. According to the present study OEO may have the antidepressant-like activity but have no effect on the stress-induced TLR-2/4 upregulation.

A novel synthesis of a new thorium (IV) metal organic framework nanostructure with well controllable procedure through ultrasound assisted reverse micelle method.

Reverse micelle (RM) and ultrasound assisted reverse micelle (UARM) were applied to the synthesis of novel thorium nanostructures as metal organic frameworks (MOFs). Characterization with different techniques showed that the Th-MOF sample synthesized by UARM method had higher thermal stability (354°C), smaller mean particle size (27nm), and larger surface area (2.02×103m2/g). Besides, in this novel approach, the nucleation of crystals was found to carry out in a shorter time. The synthesis parameters of UARM method were designed by 2k-1 factorial and the process control was systematically studied using analysis of variance (ANOVA) and response surface methodology (RSM). ANOVA showed that various factors, including surfactant content, ultrasound duration, temperature, ultrasound power, and interaction between these factors, considerably affected different properties of the Th-MOF samples. According to the 2k-1 factorial design, the determination coefficient (R2) of the model is 0.999, with no significant lack of fit. The Fvalue of 5432, implied that the model was highly significant and adequate to represent the relationship between the responses and the independent variables, also the large R-adjusted value indicates a good relationship between the experimental data and the fitted model. RSM predicted that it would be possible to produce Th-MOF samples with the thermal stability of 407°C, mean particle size of 13nm, and surface area of 2.20×103m2/g. The mechanism controlling the Th-MOF properties was considerably different from the conventional mechanisms. Moreover, the MOF sample synthesized using UARM exhibited higher capacity for nitrogen adsorption as a result of larger pore sizes. It is believed that the UARM method and systematic studies developed in the present work can be considered as a new strategy for their application in other nanoscale MOF samples.

Ag-4-ATP-MWCNT electrode modified with dsDNA as label-free electrochemical sensor for the detection of daunorubicin anticancer drug.

This paper describes the synthesis of Ag-4-ATP-MWCNT nanocomposite and its use as a modifier of working electrode. The surface of the electrochemical Ag-4-ATP-MWCNT electrode was modified with a double-stranded DNA (dsDNA) to detect daunorubicin-DNA interactions. Differential pulse voltammetry was applied to develop an electroanalytical procedure for the determination of daunorubicin and evaluate its interaction with dsDNA immobilized on the electrode surface. After the optimization of operational parameters, the linear dependence of the peak current on the daunorubicin concentration was observed in the range of 0.10×10-8 to 1.00×10-5molL-1, with the detection and quantification limits of 3.00×10-10 and 1.00×10-9molL-1, respectively. The proposed biosensor was successfully applied to validate its capability for the determination of daunorubicin in human serum and urine samples.

Cytotoxic Effect of Thymus caramanicus Jalas on Human Oral Epidermoid Carcinoma KB Cells.

Identifying new chemotherapeutic agents with fewer side effects is a major concern for scientists today. Thymus caramanicus Jalas (Lamiaceae family) is one of the species of Thymus that grows wild in different regions of Iran. Traditionally, leaves of this plant are used in the treatment of diabetes, arthritis and cancer. Here was investigated the cytotoxic property of Thymus caramanicus essential oil and extract in human oral epidermoid carcinoma KB cells. Cell viability was measured by MTT and neutral red assays. The cells were exposed to different concentrations of essential oil (0.05-1 µL/mL) and extract (25-150 µg/mL) for 24 h. Doxorubicin was used as anticancer control drug. The data showed that the essential oil (IC50=0.44 µL/mL) and extract (IC50=105 µg/mL) induce potent cytotoxic property. Surprisingly, cytotoxic effects of essential oil and extract of this plant on KB cancer cells were greater than those on normal gingival HGF1-PI1 cell line. In addition, Thymus caramanicus could potentiate the effect of doxorubicin in sub-effective concentrations. The results of the present study indicate that essential oils and extracts of Thymus caramanicus have potential anti-proliferative property on KB cells and can be used as pharmaceutical case study for oral cancer treatments.

Cytotoxic Effect of Thymus caramanicus Jalas on Human Oral Epidermoid Carcinoma KB Cells

Abstract Identifying new chemotherapeutic agents with fewer side effects is a major concern for scientists today. Thymus caramanicus Jalas (Lamiaceae family) is one of the species of Thymus that grows wild in different regions of Iran. Traditionally, leaves of this plant are used in the treatment of diabetes, arthritis and cancer. Here was investigated the cytotoxic property of Thymus caramanicus essential oil and extract in human oral epidermoid carcinoma KB cells. Cell viability was measured by MTT and neutral red assays. The cells were exposed to different concentrations of essential oil (0.05-1 µL/mL) and extract (25-150 µg/mL) for 24 h. Doxorubicin was used as anticancer control drug. The data showed that the essential oil (IC50=0.44 µL/mL) and extract (IC50=105 µg/mL) induce potent cytotoxic property. Surprisingly, cytotoxic effects of essential oil and extract of this plant on KB cancer cells were greater than those on normal gingival HGF1-PI1 cell line. In addition, Thymus caramanicus could potentiate the effect of doxorubicin in sub-effective concentrations. The results of the present study indicate that essential oils and extracts of Thymus caramanicus have potential anti-proliferative property on KB cells and can be used as pharmaceutical case study for oral cancer treatments.

Resumo A identificação de novos agentes quimioterápicos com menos efeitos colaterais é uma grande preocupação para os cientistas de hoje. Thymus caramanicus Jalas (família Lamiaceae) é uma das espécies de Thymus que cresce selvagem em diferentes regiões do Irã. Tradicionalmente, as folhas desta planta são utilizados no tratamento da diabetes, artrite e câncer. Aqui investigamos a propriedade citotóxica do óleo essencial e extrato de Thymus caramanicus em células da linhagem celular tumoral humana de carcinoma epidermóide de boca (KB). A viabilidade celular foi medida por ensaios MTT e vermelho neutro. As células foram expostas a diferentes concentrações de óleo essencial (0,05-1 μL/mL) e extrato (25-150 μg/mL) durante 24 h. A doxorrubicina foi utilizada como droga de controle anticâncer. Os dados mostraram que o óleo essencial (IC50 = 0,44 μL/mL) e o extrato (IC50 = 105 μg/mL) induzem uma potente propriedade citotóxica. Surpreendentemente, os efeitos citotóxicos de óleo essencial e extrato desta planta sobre células cancerígenas KB foram maiores que sobre a linhagem celular gengival normal HGF1-PI1. Além disso, Thymus caramanicus poderia potencializar o efeito da doxorrubicina em concentrações sub-efetivas. Os resultados do presente estudo indicam que óleos essenciais e extratos de Thymus caramanicus têm potenciais propriedades anti-proliferativas sobre células KB e podem ser usado como estudos de caso farmacêuticos para tratamentos de câncer bucal

Electrospun composite nanofibers of poly vinyl pyrrolidone and zinc oxide nanoparticles modified carbon paste electrode for electrochemical detection of curcumin.

A simple and novel ferrocene-nanofiber carbon paste electrode was developed to determine curcumin in a phosphate buffer solution at pH=8. ZnO nanoparticles were produced via a sonochemical process and composite nanofibers of PVP/ZnO were prepared by electrospinning. The characterization was performed by SEM, XRD and IR. The results suggest that the electrospun composite nanofibers having a large surface area promote electron transfer for the oxidation of curcumin and hence the FCNFCPE exhibits high electrocatalytic activity and performs well in regard to the oxidation of curcumin. The proposed method was successfully applied for measurement of curcumin in urine and turmeric as real samples.

Extraction and preconcentration of hemin from human blood serum and breast cancer supernatant.

A green, facile, fast, and sensitive liquid-phase microextraction method is presented for the extraction and preconcentration of hemin in the presence of free iron ions prior to flame atomic absorption spectroscopic determination. In this technique, an anion-functionalized task-specific ionic liquid is used as the extracting solvent. The interface between the extracting solvent and the bulk aqueous phase containing hemin is enormously enlarged by dispersing the ionic liquid to the aqueous phase with the help of ultrasound radiation. Hemin is selectively extracted into the ionic liquid after interaction with the functional group of the ionic liquid. Then, the concentration of the extracted hemin is determined through the absorbance of the iron ions contained in the hemin structure using flame atomic absorption spectroscopy. Different experimental parameters affecting the extraction efficiency have been optimized. Under the optimized conditions, the proposed method has a hemin concentration linear range of 0.020-0.80 mg/L with a detection limit of 0.0080 mg/L. This method has been successfully applied to the extraction and determination of hemin in human serum and supernatant samples.

Study of disbudding goat kids following injection of clove oil essence in horn bud region.

This study was performed to evaluate the efficacy of injection of essential oil of Eugenia caryophyllata in the kid horn buds, as a new chemical technique for disbudding. Five-day-old healthy goat kids from both sexes (n = 16) were divided randomly into 4 equal groups. In groups 1, 2 and 3, 0.2 mL of clove essence and in group 4 (control) 0.2 mL of normal saline was injected into the left horn bud of goat kids. Right horn bud in all kids was considered to ensure that they are horned. During the study, the rate of horn growth were evaluated in determined time intervals between groups 1 and 4. Tissue samples were taken from right and left horn bud in groups 2 and 3, at five and ten days after clove essence injection, for microscopic study. The results of the study showed that the clove essence stopped horn growth, whereas there was no significant difference in horn growth rate between left and right horns after injection of normal saline, in group 4. Histopathological study showed that injection of clove essence caused complete necrosis of epidermis and underlying dermis with collagenolysis in horn bud tissues, 5 days after injection and then progress in healing process was observed after 10 days. According to the results of this study, it can be concluded that the injection of clove essence is an effective method to stop horn growth without any undesirable effects on clinical parameters in goat kids.

Spectrofluorimetric determination of melatonin in kernels of four different Pistacia varieties after ultrasound-assisted solid-liquid extraction.

Melatonin is normally consumed to regulate the body's biological cycle. However it also has therapeutic properties, such as anti-tumor, anti-aging and protects the immune system. There are some reports on the presence of melatonin in edible kernels such as walnuts, but the extraction of melatonin from pistachio kernels is reported here for the first time. For this, the methanolic extract of pistachio kernels was exposed to gas chromatography/mass spectrometry analysis which confirmed the presence of melatonin. A fluorescence-based method was applied for the determination of melatonin in different extracts. When excited at λ=275 nm, the fluorescence emission intensity of melatonin was measured at λ=366 nm. Ultrasound-assisted solid-liquid extraction was used for the extraction of melatonin from pistachio kernels prior to fluorimetric determination. To achieve the highest extraction recovery, the main parameters affecting the extraction efficiency such as extracting solvent type and volume, temperature, sonication time and pH were evaluated. Under the optimized conditions, a linear dependence of fluorescence intensity on melatonin concentration was observed in the range of 0.0040-0.160 µg mL(-1), with a detection limit of 0.0036 µg mL(-1). This method was applied successfully for measuring and comparing the melatonin content in the kernels of four different varieties of Pistacia including Ahmad Aghaei, Akbari, Kalle Qouchi and Fandoghi. In addition, the results obtained were compared with those obtained using GC/MS. A good agreement was observed indicating the reliability of the proposed method.

Effects of zinc supplementation on efficacy of antidepressant therapy, inflammatory cytokines, and brain-derived neurotrophic factor in patients with major depression.

OBJECTIVE: Zinc is found in abundance in the human brain. Patients with depression may have decreased consumption of food sources rich in zinc, and zinc supplementation may have a potential influence on depressive symptoms. However, clinical trials on the effect of zinc supplementation in depression are limited. The objective of the present study was to determine the effect of zinc supplementation on efficacy of antidepressant therapy. Furthermore, the effect of zinc on plasma levels of interleukin-6 (IL-6), tumor necrosis factor (TNF-α), and brain-derived neurotrophic factor-a (BDNF-a) were assessed. DESIGN: A single-center, randomized, double-blind, placebo-controlled trial of zinc supplementation was conducted in patients with DSM-IV major depression. Forty-four patients of both sexes aged 18-55 years were recruited for this study from a university hospital. The zinc-supplemented group received zinc sulfate (25 mg elemental Zn/day) orally in addition to their selective serotonin reuptake inhibitor antidepressants for 12 weeks. Symptoms were evaluated using the Hamilton Depression Rating Scale (HDRS) on arrival, weeks 6 and 12. Plasma levels of IL-6, TNF-α and BDNF-a were measured at baseline and at the end of study. RESULTS: Twenty patients in zinc group and 17 patients in placebo groups completed the study. At baseline, there were no significant differences in any variable between the patients allocated to receive placebo and those taking zinc supplement. Zinc supplementation significantly reduced HDRS compared to placebo (P < 0.01 at 12th week). No significant differences were observed in plasma levels of IL-6, TNF-α, and BDNF-a between zinc-supplemented and placebo-supplemented group. CONCLUSION: Zinc supplementation in conjunction with antidepressant drugs might be beneficial for reducing depressive symptoms. However, its effect does not appear to be mediated through impact of zinc on inflammatory processes.

Comparison of the essential oil content and composition of the spathe, buds and pollen of Phoenix dactylifera.

Several medicinal applications have been reported for different components of date palm. The inflorescence of the male date tree is composed of spathe that surrounds many buds containing pollen. In this study, a comparison between the content and composition of the essential oils obtained from these three components of an inflorescence was made. After obtaining each oil using hydro-distillation method, the oil yield was measured as the weight ratio of the oil to the distilled sample (w/w %) and the chemical composition of the oil was determined by gas chromatography-mass spectrometry analysis. It was observed that the pollen possessed the most oil content (1.47%) composed of 68.04% oleic acid, whereas the content of this fatty acid in the spathe and bud oils was found to be less than 0.05% and 5.65%, respectively. Spathe oil was dominated by 3,4-dimethoxytoluene (52.90%) while the main constituent of the bud oil was trans-caryophyllene (44.20%).

Flame atomic absorption determination of trace amounts of cadmium after preconcentration using a thiol-containing task-specific ionic liquid.

Dispersive liquid-liquid microextraction (DLLME) based on a task-specific ionic liquid (TSIL) was developed for the extraction and preconcentration of trace amounts of cadmium from aqueous samples, followed by flame atomic absorption spectrometry (FAAS) determination. In the proposed approach, cadmium ions are extracted from aqueous samples using small volumes of trioctylmethylammonium thiosalicylate (TOMATS) dissolved in acetone. TOMATS is a thiol-containing TSIL that can form metal thiolate complexes due to the chelating effect of the ortho-positioned carboxylate group relative to the thiol functionality. The main parameters affecting the performance of DLLME based on TSIL, such as pH, amount of TOMATS, extraction time, injection volume, salt addition, and centrifugation time, were optimized. Under optimum conditions, an LOD of 1.16 ng/mL and a good RSD of 1.8% at 60.0 ng/mL were obtained (n=7). The proposed method was applied to tap water, wastewater, well water, and milk samples. The results showed that DLLME based on TSIL combined with FAAS is a rapid, simple, sensitive, selective, low cost, volatile organic solvent-free, and efficient analytical method for the separation and determination of trace amounts of cadmium ions.

Flame atomic absorption spectrometric determination of trace amounts of nickel after extraction and preconcentration onto natural modified analcime zeolite loaded with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol.

Nickel is a moderately toxic element compared with other transition metals. However, inhalation of nickel and its compounds leads to serious problems, including cancer of the respiratory system and a skin disorder, nickel-eczema. Thus, attention has focused on the toxicity of nickel at low concentrations, and the development of reliable, analytical approaches for the determination of trace amounts of nickel is needed. This paper describes a simple, rapid, and sensitive flame atomic absorption spectrometric method for the determination of trace amounts of nickel in various samples after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex on a modified Analcime column in the pH range of 7.5-10.5. The retained analyte on the Analcime is recovered with 5.0 mL 2 M nitric acid and determined by flame atomic absorption spectrometry. The detection limit is 20 ng/mL, and the calibration curve is linear for analyte concentrations in the range of 0.1-8 microg/mL final solution, with a correlation coefficient of 0.9993. Eight replicate determinations of nickel at 2 microg/mL in the final solution gave an absorbance of 0.1222, with a relative standard deviation (RSD) of +/-1.2%. The interference of a large number of anions and cations was studied, and the proposed method was used for the determination of nickel in various standard reference samples. The accuracy of the proposed method was evaluated by analyzing standard reference samples, and the results were satisfactory (recoveries of >96%; RSD of <3.5%).

Natural analcime zeolite modified with 5-Br-PADAP for the preconcentration and anodic stripping voltammetric determination of trace amount of cadmium.

A procedure for separation and preconcentration of trace amounts of cadmium has been proposed. A column of analcime zeolite modified with benzyldimethyltetradecylammonium chloride and loaded with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) was used for retention of cadmium. The cadmium was quantitatively retained on the column at pH approximately 9 and was recovered from column with 5 ml of 2 M nitric acid with a preconcentration factor of 140. Anodic stripping differential pulse voltammetry was used for determination of cadmium. A 0.05 ng/ml detection limit for the preconcentration of aqueous solution of cadmium was obtained. The relative standard deviation (RSD) for eight replicate determinations at the 1 microg/ml cadmium levels was 0.31% (calculated with the peak height obtained). The calibration graph using the preconcentration system was linear from 0.01 to 150 microg/ml in final solution with a correlation coefficient of 0.9997. For optimization of conditions, various parameters such as the effect of pH, flow rate, instrumental conditions and interference of number of ions, were studied in detail. This method was successfully applied for determination of cadmium in various complex samples.