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1.
As selenium is an important part of the antioxidant enzymes and also because there are several studies suggesting a possible link between cancer and selenium deficiency, this paper presents a spectrophotometric method for the assay of Se(IV), using N,N-diethyl-p-phenylenediamine monohydrochloride as reagent. The proposed method is based on the reaction between the selenium and potassium iodide in low acidic medium, when iodine is released. This last product will further oxidise the new reagent. The final obtained product is strongly coloured in red and has an absorption maximum at 552 nm and molar extinction coefficient (ε) of 6.1?×?104 L mol?1 cm?1. The optimum working conditions were established, and the developed method was validated, being characterised by a good linearity (in the range of 0.5–3.0 μg/mL), a limit of detection (0.0573 μg/mL) and a limit of quantification (0.1737 μg/mL). At the same time, the repeatability, the precision of the method and the accuracy were established. The proposed and validated method was applied with good results for the determination of Se(IV) in spring and bottled water from Iasi and also in pharmaceutical and cosmetic products.  相似文献   

2.
A simple, rapid, and efficient dispersive liquid–liquid microextraction method, followed by UV–Vis spectrophotometry was developed for the preconcentration and determination of Pd ions in water samples. Pd ions react with α-furildioxime (chelating agent) to form a hydrophobic complex. Various parameters were altered to study and optimize their effects on the extraction efficiency, such as pH, ligand concentration, the type and volume of extraction and dispersive solvents, extraction time, and salt concentration. Under optimized conditions, the method exhibited an enrichment factor (C org/C aq) of 25 and recovery more than 98 % within a very short extraction time. The linearity of the method ranged from 10 to 200 μg?L?1. The limit of detection was 1.1 μg?L?1. The relative standard deviation for the concentration of 100 μg?L?1 of Pd was 2.3 % (n?=?10). Finally, the developed method was successfully applied to the extraction and determination of Pd in tap, river, mineral, and sea water samples.  相似文献   

3.
In this study, an ultra-sensitive and highly selective, rapid flow-injection spectrophotometric method for the determination of iron (II) and total iron has been proposed. The method was based on the reaction between iron (II) and 2′, 3, 4′, 5, 7-pentahydroxyflavone in slightly acidic solution with a strong absorption at 415 nm. The carrier solution used was 1?×?10?5 M 2′, 3, 4′, 5, 7-pentahydroxyflavone in 0.1 M HAc/Ac? buffer solution at pH 4.5. Parameters that affect simultaneously the determination of iron (II) and interfering ions were tested. The relative standard deviation for the determination of 50 μg L?1 iron (II) was 0.85 % (n?=?10), and the limit of detection (blank signal plus three times the standard deviation of the blank) was 3 μg L?1, both based on injection volumes of 20 μL. The method has been successfully applied to the determination of iron (II) and total iron in water samples and ore samples. The method was verified by analysing a certified reference material Zn/Al/Cu 43XZ3F.  相似文献   

4.
A simple, sensitive, and accurate UV spectrophotometric method has been developed for the determination of nickel in synthetic mixture and water samples. The method is based on the complexation reaction of nickel ion with cefixime, thus leading to the formation of Ni–cefixime complex in ethanol-distilled water medium at room temperature. The complex showed the maximum absorption wavelength at 332 nm. Beer’s law is obeyed in the working concentration range of 0.447–4.019 μg?mL?1 with apparent molar absorptivity of 7.314?×?103?L?mol?1?cm?1 and Sandell’s sensitivity of 0.008 μg/cm2/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.016 and 0.054 μg?mL?1, respectively. The factors such as cefixime concentration and solvent affecting the complexation reaction were carefully studied and optimized. The method is validated as per the International Conference on Harmonisation guideline. The method is successfully applied to the determination of Ni(II) in synthetic mixture and wadi water samples collected from Al Rustaq. The same water samples are also analyzed by atomic absorption spectrophotometry. Both methods determined the amount of Ni(II) in water sample and found to be approximately the same.  相似文献   

5.
This study reports the feasibility of applying directly suspended liquid-phase microextraction (DSLPME)-gas chromatography detection for the pre-concentration and determination of low levels of eight polychlorinated biphenyls (PCBs) in aqueous samples. The technique requires minimal sample preparation, analysis time and solvent consumption and represents significant advantages over conventional analytical methods. The experimental parameters such as salt content, sample temperature, stirring rate, extraction time, micro-drop volume and breakthrough volume were investigated and found to have significant influences on DSLPME. Under the optimal experimental conditions, the enrichment factor ranged from 578 to 729, and the recovery was above 93 %. Calibration curves possessed good linearity (R 2?>?0.99) over a wide concentration range of 0.1–10.0 μg L?1 with limits of detection ranging from 0.01 to 0.07 μg L?1. The relative standard deviations for 1.0 μg L?1 of PCBs in water by using internal standard were in the range 2–14 % (n?=?3). The proposed simple, accurate and sensitive analytical method was applied successfully to the determination of trace amounts of PCBs in water samples.  相似文献   

6.
Monitoring of heavy metals was conducted in the Yamuna River considering bioaccumulation factor, exposure concentration, and human health implications which showed contamination levels of copper (Cu), lead (Pb), nickel (Ni), and chromium (Cr) and their dispersion patterns along the river. Largest concentration of Pb in river water was 392 μg L?1; Cu was 392 μg L?1 at the extreme downstream, Allahabad and Ni was 146 μg L?1 at midstream, Agra. Largest concentration of Cu was 617 μg kg?1, Ni 1,621 μg kg?1 at midstream while Pb was 1,214 μg kg?1 at Allahabad in surface sediment. The bioconcentration of Cu, Pb, Ni, and Cr was observed where the largest accumulation of Pb was 2.29 μg kg?1 in Oreochromis niloticus and 1.55 μg kg?1 in Cyprinus carpio invaded at Allahabad while largest concentration of Ni was 174 μg kg?1 in O. niloticus and 124 μg kg?1 in C. carpio in the midstream of the river. The calculated values of hazard index (HI) for Pb was found more than one which indicated human health concern. Carcinogenic risk value for Ni was again high i.e., 17.02?×?10?4 which was larger than all other metals studied. The results of this study indicated bioconcentration in fish due to their exposures to heavy metals from different routes which had human health risk implications. Thus, regular environmental monitoring of heavy metal contamination in fish is advocated for assessing food safety since health risk may be associated with the consumption of fish contaminated through exposure to a degraded environment.  相似文献   

7.
The aim of the present work is the assessment of a new sorbent, prepared using silica gel coated with a pyrimidine derivative (allyl 6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate), for extraction and preconcentration trace amount of lead from different samples prior to determination by flame atomic absorption spectrometry. Common coexisting ions did not interfere with the separation and determination of lead at pH?6, so that lead ion completely adsorbed on the column. The limit of detection based on three times the standard deviation of the blank was found to be 0.53 ng?mL?1 in original solution. Obtained sorption capacity for 1 g sorbent was 5.0 mg Pb. The linearity was maintained in the concentration range of 0.1–30.0 ng?mL?1 for the concentrated solution. Eight replicate determinations of 2.0 μg?mL?1 of lead in the final solution gave relative standard deviation of ±2.6 %. The proposed method was successfully applied to the determination trace amounts of lead in the environmental samples such as carrot, rice, zardchoobe, and real water samples.  相似文献   

8.
The dissolved labile and labile particulate fractions (LPF) of Cu and Zn were analyzed during different seasons and salinity conditions in estuarine waters of marina, port, and shipyard areas in the southern region of the Patos Lagoon (RS, Brazil). The dissolved labile concentration was determined using the diffusive gradients in thin films technique (DGT). DGT devices were deployed in seven locations of the estuary for 72 h and the physicochemical parameters were also measured. The LPF of Cu and Zn was determined by daily filtering of water samples. Seasonal variation of DGT–Cu concentrations was only significant (p?<?0.05) at one shipyard area, while DGT–Zn was significant (p?<?0.05) in every locations. The LPF of Cu and Zn concentrations demonstrated seasonal and spatial variability in all locations, mainly at shipyard areas during high salinity conditions. In general, except the control location, the sampling locations showed mean variations of 0.11–0.45 μg?L?1 for DGT–Cu, 0.89–9.96 μg?L?1 for DGT–Zn, 0.65–3.69 μg?g?1 for LPF–Cu, and 1.35–10.87 μg?g?1 for LPF–Zn. Shipyard areas demonstrated the most expressive values of labile Cu and Zn in both fractions. Strong relationship between DGT–Zn and LPF–Zn was found suggesting that the DGT–Zn fraction originates from the suspended particulate matter. Water salinity and suspended particulate matter content indicated their importance for the control of the labile concentrations of Cu and Zn in the water column. These parameters must be taken into consideration for comparison among labile metals in estuaries.  相似文献   

9.
A new complexing agent, 2-((2-((1H-benzo[d]imidazole-2yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazole (BIMPI), was used in cloud point extraction and applied for selective pre-concentration of trace amounts of cadmium in cigarette samples. Cadmium was complexed with BIMPI in a buffer solution (pH?=?10) using Triton X-114 as surfactant and quantitatively extracted into a small volume of the surfactant-rich phase after centrifugation. Under optimized conditions (pH?=?10.0, 0.8?×?10?4?mol?L?1 BIMPI and 0.08 % (w/v) Triton X-114), calibration graph was linear in the range of 34.0–1,670.0 μg?L?1. The proposed method was applied to the determination of Cd in various cigarette (tobacco) samples which gave satisfactory results.  相似文献   

10.
The prevalence of fluorosis is mainly due to the consumption of more fluoride (F?1) through drinking water, vegetables, and crops. The objective of the study was mapping of F?1 endemic area of Newai Tehsil, Tonk district, Rajasthan, India. For the present study, water, soil (0–45 cm), and vegetation samples were collected from 17 villages. Fluoride concentration in water samples ranged from 0.3 to 9.8 mg/l. Out of 17 villages studied, the amounts of F?1 content of eight villages were found to exceed the permissible limits. Labile F?1 content and total F?1 content in soil samples ranges 11.00–70.05 mg/l and 50.3–179.63 μg g?1, respectively. F?1 content in tree species was found in this order Azadirachta indica 47.3255.76 μg g?1 > Prosopis juliflora 40.16–49.63 μg g?1 > Acacia tortilis 34.39–43.60 μg g?1. While in case of leafy vegetables, F?1 content order was Chenopodium album 54.23–98.42 μg g?1 > Spinacea oleracea 30.41–64.09 μg g?1 > Mentha arvensis 35.4851.97 μg g?1. The order of F?1 content in crops was found as 41.04 μg g?1 Pennisetum glaucum > 13.61 μg g?1 Brassica juncea > 7.98 μg g?1 Triticum sativum in Krishi Vigyan Kendra (KVK) farms. Among vegetation, the leafy vegetables have more F?1 content. From the results, it is suggested that the people of KVK farms should avoid the use of highly F?1 containing water for irrigation and drinking purpose. It has been recommended to the government authority to take serious steps to supply drinking water with low F?1 concentration for the fluorosis affected villages. Further, grow more F?1 hyperaccumulator plants in F?1 endemic areas to lower the F?1 content of the soils.  相似文献   

11.
The dissipation kinetics and method for estimation of residues of chlorpyrifos and lambda-cyhalothrin in cardamom were studied and developed. The limit of detection and limit of quantitation arrived for the compounds were 0.01 and 0.025 μg?g?1, respectively. Gas chromatographic response of chlorpyrifos and lambda-cyhalothrin residues was linear in the range of 0.01–0.50 μg?g?1 and the mean recovery obtained was 97.3 % for chlorpyrifos and 98.9 % for lambda-cyhalothrin with satisfactory relative standard deviation values. The mean initial residues of chlorpyrifos applied at a concentration of 0.05 % in cardamom was 2.5 μg?g?1 and the residue was 8.1 μg?g?1 after processing, with a processing factor of 3.24, while lambda-cyhalothrin when applied at 0.0025 % resulted in initial residues of 1.63 μg?g?1 that magnified to 4.86 μg?g?1 on curing, with a processing factor of 2.98. The half-life of chlorpyrifos was in the range of 5.1–5.24 days while that of lambda-cyhalothrin was in the range of 4.40–4.55 days. The processing factor arrived at in the above experiment lead to the conclusion that the residues of chlorpyrifos got magnified to 3.24–3.68 times and that of lambda-cyhalothrin got magnified to 2.98–3.46 times of initial residues, consequent to loss of weight due to dehydration during curing.  相似文献   

12.
Exposure to arsenic in arsenic endemic areas is most remarkable environmental health challenges. Although effects of arsenic contamination are well established, reports are unavailable on probable seasonal variation due to changes of food habit depending on winter and summer seasons, especially for endemic regions of Nadia district, West Bengal. Complete 24-h diets, drinking–cooking water, first morning voided urine samples, and diet history were analyzed on 25 volunteers in arsenic endemic Chakdah block of Nadia district, once in summer followed by once in winter from the same participants. Results depicted no seasonal variation of body weight and body mass index. Arsenic concentration of source drinking and cooking water decreased (p?=?0.04) from 26 μg L?1 in summer to 6 μg L?1 in winter season. We recorded a seasonal decrease of water intake in male (3.8 and 2.5 L day ?1) and female (2.6 and 1.2 L day?1) participants from summer to winter. Arsenic intake through drinking water decreased (p?=?0.04) in winter (29 μg day?1) than in summer (100 μg day?1), and urinary arsenic concentration decreased (p?=?0.018) in winter (41 μg L?1) than in summer (69 μg L?1). Dietary arsenic intake remained unchanged (p?=?0.24) over the seasons. Hence, we can infer that human health risk assessment from arsenic needs an insight over temporal scale.  相似文献   

13.
Concentrations of 16 priority polycyclic aromatic hydrocarbons (PAHs) were measured in 28 surface soils samples collected from Urumqi, northwest China, for examination of distributions, source contributions, and potential health effects. The results indicated that the sum of 16 PAHs concentration ranged from 331 to 15,799 μg?kg?1 (dw) in soils, with a mean of 5,018?±?4,896 μg?kg?1 (n?=?28). The sum of seven carPAHs concentration ranged from 4 to 1,879 μg?kg?1 (dw; n?=?28). The highest ∑PAHs concentrations were found at roadsides and industrial sites, followed by those at parks, rural areas, and business/residential areas. Coal combustion, emission of diesel and gasoline from vehicles, and petroleum source were four sources of PAHs as determined by PMF analysis, which contributed 51.19, 19.02, 18.35, and 11.42 % to the PAH sources, respectively. Excellent coefficients of correlation between the measured and predicted PAHs concentrations suggested that the PMF model was very effective to estimate sources of PAHs in soils. Incremental lifetime cancer risk values at the 95th percentile due to human exposure to surface soils PAHs in Urumqi were 2.02?×?10?6 for children and 2.72?×?10?5 for adults. The results suggested that the current PAHs levels in soils from Urumqi were pervasive and moderately carcinogenic to children and adults.  相似文献   

14.
The determination of mercury in crude oil and petroleum products is particularly difficult due to the volatile nature of both mercury and the matrix, which may lead to significant loss of the analyte. A simple extraction method for total mercury has been developed to determine total mercury in crude oil using cold vapor atomic fluorescence spectrometry. The homogenized crude oil sample was diluted to 5, 10, and 20 % (w/w) in toluene. The diluted crude oil samples were spiked with 10 and 40 μg/kg (w/w). The samples were extracted using an oxidant/acid solution, BrCl/HCl. The mercury was extracted into the aqueous phase; the ionic mercury was then reduced to volatile elemental mercury (Hg0) by stannous chloride (SnCl2). The mercury vapor was detected by Merlin cold vapor atomic fluorescence spectrometry at a 253.7-nm wavelength. The average recoveries for mercury in spiked diluted crude oil (10 and 40 μg/kg, w/w) were between 96 and 103 %, respectively, in 5 and 10 % spiked diluted crude oil. Whereas, low recoveries (<50 %) were recorded in 20 % diluted spiked crude oil. The method detection limit was calculated as t (0.01)(n ? 1)?×?SD where t is the student's value for 99 % confidence level and standard deviation estimate with n???1 degrees of freedom. The method detection limit was found to be 0.38 μg/kg based on 5 g of diluted crude oil sample. The method is sensitive enough to determine low levels of mercury in crude oil.  相似文献   

15.
The aim of this study was to evaluate the incidence of total aflatoxin (AF), ochratoxin A, T-2 toxin, deoxynivalenol (DON), zearalenone (ZEA), and fumonisin (FB) in dairy cattle, beef cattle, and lamb–calf feeds. A total of 180 dairy cattle, beef cattle, and lamb–calf feeds (60 samples each) were randomly collected from farms, feed mills, and villages in Burdur province, between September 2006 and August 2007. All samples were analyzed by the competitive Enzyme Linked Immuno Sorbent Assay (ELISA). The most frequent mycotoxin detected was total AF, which was found in 108 samples (60 %) in concentrations ranging from 3.82 to 116.83 μg?kg?1, followed by DON that was detected in 87 samples (48.3 %), in concentrations ranging from 18.50 to 500 μg?kg?1. Ochratoxin A (OTA), T-2 toxin, ZEA, and FB were found in 84 (46.7 %), 85 (47.2 %), 57 (31.7 %), and 19 (10.6 %) samples, respectively, in concentrations of 1.01 to 15.85 μg?kg?1 for OTA, 3.85 to 52.36 μg?kg?1 for T-2 toxin, 2.10 to 29.30 μg?kg?1 for ZEA, and 2.69 to 4.96 mg?kg?1 for FB. It was concluded that feed samples in Burdur province were contaminated by mycotoxins, and the levels of total aflatoxin in the samples were considered a risk to animal health.  相似文献   

16.
Concentrations of trace metals in the South China Sea (SCS) were determined off the coast of Terengganu during the months of May and November 2007. The concentrations of dissolved and particulate metals were in the range of 0.019–0.194 μg/L and 50–365 μg/g, respectively, for cadmium (Cd), 0.05–0.45 μg/L and 38–3,570 μg/g for chromium (Cr), 0.05–3.54 μg/L and 21–1,947 μg/g for manganese (Mn), and 0.03–0.49 μg/L and 2–56,982 μg/g for lead (Pb). The order of mean log K D found was Cd?>?Cr?>?Pb?>?Mn. The study suggests that the primary sources of these metals are discharges from the rivers which drain into the SCS, in particular the Dungun River, which flows in close proximity to agricultural areas and petrochemical industries. During the northeast monsoon, levels of particulate metals in the bottom water samples near the shore were found to be much higher than during the dry season, the probable result of re-suspension of the metals from the bottom sediments.  相似文献   

17.
With the aim of knowing Hg distribution in selected tissues of myliobatid stingrays and assessing health risk to Mexican population, Hg concentration was determined in the muscle and liver of four ray species. Total Hg levels were determined by cold vapor atomic absorption spectrophotometry. With respect to the muscle, devil rays (Mobula spp.) showed lower Hg levels (<0.22 μg g?1) than Rhinoptera steindachneri (0.37?±?0.25 μg g-1 wet weight). In the case of the liver, the highest Hg concentration was found in Mobula japanica (0.22?±?0.01 μg g?1). Hg levels in the muscle and liver varied according to the species; in some case, the liver accumulated more Hg than the muscle and the opposite pattern in other cases. R. steindachneri showed a significant difference between both tissues. No significant differences of Hg levels between males and females and between juveniles and adult specimens of R. steindachneri were found. Positive correlation between Hg concentrations and disc width and total weight was not significant for R. steindachneri (Rs?<?0.36, p?>?0.05). Batoids showed Hg values below the Mexican (NOM-027-SSA1-1993) limits (1.0 μg g?1) in fishes for human consumption. The species with the highest potential of Hg transfer to human population is R. steindachneri; however, an adult (70 kg) could consume approximately 943 g per week without representing a health risk. Nevertheless, further and continuous monitoring is needed since batoids support an important fishery in Mexican waters, being a food resource and income to coastal communities.  相似文献   

18.
The toxicity of mercury, zinc and copper on sperm viability, fertilisation and embryogenesis of Ruditapes decussatus was examined. Cu did not affect sperm viability at all the concentrations tested. Conversely, the Zn and Hg significantly (P?<?0.01) reduced sperm viability only at the highest concentration (respectively 512 and 256 μg/l). Cu caused a significant decrease (p?<?0.05) of less than 6% in the fertilisation rate at 128 μg/l and Zn of up to 13% at 64 μg/l. Hg significantly (p?<?0.01) inhibited fertilisation at concentrations as low as 32 μg/l. The median effective concentrations (EC50) reducing rates of embryogenesis by 50% were 21.1 μg Hg/l (0.1 μM), 46.3 μg Cu/l (0.72 μM) and 43.4 μg Zn/l. Therefore, Hg is up to seven times more toxic than Cu (on a molar basis). Ecotoxicity of mercury on larvae survival was also assessed in this work. Result showed a significant (p?<?0.05) reduction of survival after exposure to 4 and 12 μg/l of Hg. The fertilisation rate and embryogenesis were the most sensitive endpoints, although the latter is more advisable for routine assessment of seawater quality because of its greater sensibility.  相似文献   

19.
This work proposes a procedure for the determination of total selenium content in shellfish after digestion of samples in block using cold finger system and detection using atomic fluorescent spectrometry coupled hydride generation (HG AFS). The optimal conditions for HG such as effect and volume of prereduction KBr 10 % (m/v) (1.0 and 2.0 ml) and concentration of hydrochloric acid (3.0 and 6.0 mol L?1) were evaluated. The best results were obtained using 3 mL of HCl (6 mol L?1) and 1 mL of KBr 10 % (m/v), followed by 30 min of prereduction for the volume of 1 mL of the digested sample. The precision and accuracy were assessed by the analysis of the Certified Reference Material NIST 1566b. Under the optimized conditions, the detection and quantification limits were 6.06 and 21.21 μg kg?1, respectively. The developed method was applied to samples of shellfish (oysters, clams, and mussels) collected at Todos os Santos Bay, Bahia, Brazil. Selenium concentrations ranged from 0.23?±?0.02 to 3.70?±?0.27 mg kg?1 for Mytella guyanensis and Anomalocardia brasiliana, respectively. The developed method proved to be accurate, precise, cheap, fast, and could be used for monitoring Se in shellfish samples.  相似文献   

20.
This work proposes the quantification of Cr (VI) ions in natural waters in trace level, using activated alumina (Al2O3) as preconcentration support, controlled in-line dissolution of the solidified chromophore diphenylcarbazide after heat treatment and spectrophotometric detection. The manifold ensures high sensitivity of analytical response, good repeatability, and stability. In this work, optimization of experimental conditions of a flow injection system was chosen as the parameters for greater sensitivity and better selectivity. The selected optimized conditions were 0.30 mol L?1 for H2SO4 concentration, system flow rate as 0.40 mL min?1, sample injection volume of 192.50 μL, 2 min for preconcentration time, and 0.10 mol L?1 for eluent concentration. The analytical curves obtained for real sample analysis show linear range from 0.192 to 0.961 μM, linear correlation coefficient R?=?0.9997 and LOD?=?0.024 μM. The preconcentration factor of about four times was obtained through the passage of 800 μL of a standard solution containing 0.961 μM of Cr (VI) through mini-column of preconcentration followed by elution at 192.5 μL of NH4OH 0.1 mol L?1 solution. The solid chromogenic reagent presented high durability (weeks in daily use with mass of 0.0993 g) and good reproducibility in analytical signal. The reactivation of the mini-column of alumina should be executed after ten injections of eluent, using 800 μL of HCl 0.02 mol L?1 solution in flow through the same. Each cycle of injection and elution of the sample takes about 5 min on the proposed terms. Despite the length of each cycle still be high, low concentrations can be detected using a technique of relatively low cost. This is due in part, the association dissolution of the chromogenic reagent directly in the line and the preconcentration step. Another important factor is the economy of reagent chromogenic, low generation of reject contributing to better quality of the environment, and the high potential for applications to work in field.  相似文献   

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