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1.
A Varian Techtron model 63 carbon rod atomizer is used for the atomic absorption spectrometric determination of nanogram quantities of selenium. The pronounced interferences from the matrices in biological digests can be obviated by isolating selenium from sample matrices by precipitation with ascorbic acid. The precision of the determination is improved by incorporating 5000 μg Ni ml?1 in the analytical solutions. Selenium at μg g?1 and sub-μg g?1 levels in a variety of biological samples can be determined. The detection limit is 25 ng Se g?1.  相似文献   

2.
Polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs), such as DDT and analogues, hexachlorocyclohexane (HCH) isomers and hexachlorobenzene (HCB), were measured in surface soils and sediments from Eastern Romania. Thirty-nine soil samples from the forested zone, eight soil samples from a municipal waste-disposal site, and 10 sediment samples from the Bahlui River along the Iassy city were analysed using accelerated solvent extraction (ASE) and gas chromatography coupled to electron capture detection or mass spectrometry. The low mean concentrations of OCPs (11–31 and 22–84?ng?g?1 for HCHs and DDTs, respectively) and PCBs (8–43?ng?g?1) in soil samples from the forested zone suggest that contamination at most of these sites occurred predominantly through atmospheric transport from zones where these compounds were used and subsequently through atmospheric deposition. Contrarily, soil samples collected in the vicinity of a waste-disposal site near Iassy contained higher mean levels of PCBs (278?ng?g?1, range 34–1132?ng?g?1) than OCPs (6 and 101?ng?g?1 of soil for HCHs and DDTs, respectively). The sediment samples collected along the Bahlui river throughout the Iassy city revealed higher mean levels of PCBs (59?ng?g?1, range 24–158?ng?g?1) compared with OCP levels (2 and 37?ng?g?1 of soil for HCHs and DDTs, respectively). Furthermore, PCB profiles and concentrations in the sediment samples varied considerably along the river due to a wide variety of sources, such as different industries and waste sites. Although their sources are difficult to evaluate, the presence of POPs at most sites (especially at the waste-disposal site) may constitute a potential health hazard.  相似文献   

3.
Abstract

Cuccìa is a traditional Sicilian food prepared by boiling whole durum wheat kernels, in water, for many hours. This process destroys the vitamins E and B contents of crude kernels. It was rated a method to prepare the Cuccìa, preserving the vitamin content. Four varieties of durum wheat were processed comparing the traditional cooking method (TR-boiling for 5/6?hours), and an innovative one (IN-grains scarification, germination, and cooking at 50?°C for 2?hours). On soups obtained the content of biotin, niacin and α-amylase activity were determined. ANOVA showed the cooking method influences biotin and niacin content having values from 0.56 and 0.72?ng ml?1 (raw grain) and values close to 0 (TR), while only a 10% decrease (IN) respectively for both vitamins. On the contrary, α-amylase activity was reduced with IN method. The IN method combined with ancient grains, produces the soup with a good vitamin B amount.  相似文献   

4.
The distribution of 17 pharmaceuticals between water and the solid phase (sediments and soils) was studied by utilizing solid-phase extraction (SPE) and liquid chromatography?Ctandem mass spectrometry (LC-MS/MS). Two extraction procedures for soils and sediments, prior to the SPE, one based on pressurized liquid extraction (PLE) with hot water and the other on methanol/water ultrasonic extraction, were compared. Absolute recoveries were 71.2?C99.3% [relative standard deviation (RSD) <21.4%)] for water, and the method detection limits (MDLs) ranged from 0.3 to 10?ng?L?1. Recoveries were 35.4?C105.3% (RSDs <19.1%) and 42.1?C97.8% (RSDs <14%) for soil and sediment samples, respectively, using PLE and 20.2?C86.5% (RSDs <25.1%) and 30.3?C97.4% (RSDs <19.1%) using ultrasonic extraction. Fifteen of the 17 pharmaceuticals were present in the L??Albufera water at concentrations up to 17???g?L?1. Oxytetracycline and tetracycline were not detected. In sediments, only tetracycline, norfloxacin and diclofenac were not found. The other studied pharmaceuticals were present in the range from less than the method quantification limit (MQL) to 35.83?ng?g?1. Among the 17 target compounds, ofloxacin, ciprofloxacin, norfloxacin, trimethoprim, clofibric acid and diclofenac were not detected in soil samples. The average concentrations ranged from less than the MQL for ibuprofen to 34.91?ng?g?1 for tetracycline. These results indicate that pharmaceuticals could survive the wastewater treatment processes, which could lead to their dissemination in water environments.  相似文献   

5.
The method developed for determining platinum and palladium in rocks and soils is based on extraction of iodo complexes of these elements into methyl isobutyl ketone (MIBK), followed by electrothermal atomic absorption spectrometry of the extracts. The limit of detection is 10 ng g?1 for platinum and 3 ng g?1 for palladium. Analysis of the standard noble metal ore PTC-1 with recommended values of 12.7 μg g?1 for palladium and 3.0 μg g?1 for platinum gave precisions of 4.4% and 5.6%, respectively, and deviations of 5.0% and 1.2% from the recommended values. The method is applicable to the determination of both elements in a wide variety of rocks and soils.  相似文献   

6.
Selenium is determined in the ng g?1 to μg g?1 range in biological and environmental samples. A wet digestion procedure was optimized with respect to volatility losses and recovery yields, by using 75Se metabolically incorporated into rat organs. Selenium is preconcentrated from the digestion liquid by a two-step reduction with 4 M HCl and ascorbic acid. The colloidal selenium formed is adsorbed on activated carbon and filtered on a Nucleopore membrane for measurement by energy-dispersive x-ray fluorescence. Almost complete recovery was obtained, and the detection limit was 20 ng, corresponding to 10 ng g?1 for a 2-g sample. Biological reference materials were analyzed with satisfactory results, and the accuracy of the method was good.  相似文献   

7.
This paper describes an on-line sample preparation method for the simultaneous determination of 48 pesticides in grapes, baby food and wheat flour matrices. Target pesticides were selected to represent a wide variety of chemical structures and three typical matrices were selected. Turbulent flow chromatography was applied for on-line sample cleanup directly coupled to LC?CMS/MS. The aim of the method was to reduce total analysis time, eliminate manual laboratory work, provide clean extracts and achieve reproducible results. Single laboratory method validation was conducted establishing limits of detection between 0.8 and 6.0?ng?g?1 for baby food, and 0.8?C10.3?ng?g?1 for other matrices. Within-day precision values varied between 4 and 18?%, while between-day precisions were in the range 5?C22?%. Method recovery ranged from 67 to 124?%, and method accuracy was demonstrated by analysis of external quality control samples. The method was also tested on 24 different survey samples from both bio and organic origin. The method was shown to be convenient, fast and fit for purpose in meeting regulatory requirements for pesticide residue monitoring.  相似文献   

8.
Nonylphenol (NP), octylphenol (OP), nonylphenol monoethoxylate (NP1EO) and nonylphenol diethoxylate (NP2EO) are products of the biodegradation of alkylphenol polyethoxylates (AP n EO) which are used worldwide as detergents and surfactants. NP and OP are categorized as definitely endocrine disruptors. 2,4-Tert-butylphenol (BP) is extensively used for anti-oxidant of rubber and plastics. This work proposed a simple and stable method for simultaneously determining the concentration of NP, OP, BP, n-NP1EO and n-NP2EO in meat and fish, without requiring the complex pretreatments of current methods. This study used liquid extraction with acetonitrile and hexane and solid extraction using Florisil, in that order to pretreat samples. The sample solutions were analyzed to identify NP, OP, BP, n-NP1EO and n-NP2EO by HPLC with fluorescence detection. The mean recoveries were 85.3?±?3.32% for OP, 87.5?±?6.01% for BP, 90.9?±?4.72% for NP, 86.4?±?4.81% for n-NP2EO and 90.9?±?4.84% for n-NP1EO. The average coefficients of variation were about 6%. The method's detection limits were 5.4?ng?g?1 for OP, 5.2?ng?g?1 for BP, 8.9?ng?g?1 for NP, 8.7?ng?g?1 for n-NP2EO and 8.1?ng?g?1 for n-NP1EO. This work analyzed 5 kinds of usual foodstuffs of meat and fish that are frequently consumed by residents of Taiwan. All of these samples contained NP, but not detectable levels n-NP1EO. Only salmon was contaminated with n-NP2EO. The NP level was highest in cod (198.41?±?129.34?ng?g?1, wet weight). The fried chicken had the highest BP level (48.0?±?41.3?ng?g?1, wet weight), and the uncooked chicken had the highest OP level (66.6?±?53.0?ng?g?1, wet weight).  相似文献   

9.
A sensitive and robust method using solid-phase extraction and ultrasonic extraction for preconcentration followed by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS–MS) has been developed for determination of 19 biocides: eight azole fungicides (climbazole, clotrimazole, ketoconazole, miconazole, fluconazole, itraconazole, thiabendazole, and carbendazim), two insect repellents (N,N-diethyl-3-methylbenzamide (DEET), and icaridin (also known as picaridin)), three isothiazolinone antifouling agents (1,2-benzisothiazolinone (BIT), 2-n-octyl-4-isothiazolinone (OIT), and 4,5-dichloro-2-n-octyl-isothiazolinone (DCOIT)), four paraben preservatives (methylparaben, ethylparaben, propylparaben, and butylparaben), and two disinfectants (triclosan and triclocarban) in surface water, wastewater, sediment, sludge, and soil. Recovery of the target compounds from surface water, influent, effluent, sediment, sludge, and soil was mostly in the range 70–120?%, with corresponding method quantification limits ranging from 0.01 to 0.31?ng?L?1, 0.07 to 7.48?ng?L?1, 0.01 to 3.90?ng?L?1, 0.01 to 0.45?ng?g?1, 0.01 to 6.37?ng?g?1, and 0.01 to 0.73?ng?g?1, respectively. Carbendazim, climbazole, clotrimazole, methylparaben, miconazole, triclocarban, and triclosan were detected at low ng?L?1 (or ng?g?1) levels in surface water, sediment, and sludge-amended soil. Fifteen target compounds were found in influent samples, at concentrations ranging between 0.4 (thiabendazole) and 372?ng?L?1 (methylparaben). Fifteen target compounds were found in effluent samples, at concentrations ranging between 0.4 (thiabendazole) and 114?ng?L?1 (carbendazim). Ten target compounds were found in dewatered sludge samples, at concentrations ranging between 1.1 (DEET) and 887?ng?g?1 (triclocarban).  相似文献   

10.
A method for the analysis of chlorotoluenes (CTs) in soil has been developed based on ultrasonic assisted extraction with a low volume of organic solvent and determination by gas chromatography-tandem mass spectrometry (GC–MS/MS). A simultaneous clean-up on an alumina–anhydrous sodium sulphate mixture was carried out to remove soil interferences. However, an additional clean-up with graphitised carbon was needed for some very dirty samples. Several solvents were assayed and a mixture of ethyl acetate:hexane (80?:?20, v/v) was selected to carry out soil extractions. Recovery studies were performed at 0.2, 0.1, 0.05 and 0.02?ng?g?1 fortification levels, and recoveries obtained for all the compounds and concentrations were higher than 81% with standard deviations fulfilling the requirements of the IUPAC. LODs from 0.7 to 5.2?ng?kg?1 and LOQs from 2.2 to 17.5?ng?kg?1 were achieved for the analysed compounds, being pentachlorotoluene the compound with the highest limits, followed by the monochlorinated toluenes. The proposed analytical method was applied to determine CT levels in agricultural and industrial soils. These compounds were found in all the industrial soils analysed and some CTs were present in agricultural soils at lower levels.  相似文献   

11.
A column, solid phase extraction (SPE), preconcentration method was developed for determination of silver by using alumina coated with 1-((5-nitrofuran-2-yl)methylene)thiosemicarbazide and determination by flame atomic absorption spectrometry. The separation/preconcentration conditions for the quantitative recovery were investigated. At pH 2, the maximum sorption capacity of Ag+ was 7.5?mg?g?1. The linearity was maintained in the concentration range of 0.02–11.0?µg?mL?1 in the final solution or 0.14–1.10?×?104?ng?mL?1 in the original solution for silver. The preconcentration factor of 140 and relative standard deviation of ±1.4% was obtained, under optimum conditions. The limit of detection (LOD) was calculated as 0.112?ng?mL?1, based on 3σbl/m (n?=?8) in the original solutions. The proposed method was successfully applied to the determination trace amounts of silver in the environmental samples such as tea, rice and wheat flour, mint, and real water samples.  相似文献   

12.
The validation of a multi-residue method for the determination of five neonicotinoid insecticides (imidacloprid, clothianidin, acetamiprid, thiacloprid and thiamethoxam) in honeybees is described. The method involves the extraction of pesticides using acetonitrile and liquid partitioning with n-hexane. One clean-up is then performed on a florisil cartridge (1?g, 6?mL) and the extract is analysed by liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The recovery data were obtained by spiking honeybees samples free of pesticides at two concentration levels of the various neonicotinoids. The recoveries were in the range between 93.3 and 104.0% with relative standard deviation (RSD) less than 20%. The limit of quantification (LOQ) was 0.5?ng?g?1 (corresponding to 0.05?ng?bee?1) for all pesticides except for acetamiprid which was 1?ng?g?1 (corresponding to 0.1?ng?bee?1).  相似文献   

13.
With the wide range of metallic contaminants discharged in the environment, studying the human health requires a growing number of elements to be monitored in biological samples. Hair analysis has been suggested as a suitable tool for biomonitoring environmental and occupational exposure to toxic elements. This study describes a method for the determination of 10 trace elements in hair samples using ICP-QQQ-MS. Combining the power of the MS/MS high-energy Helium mode with the MS/MS O2 mass-shift mode, the method offers great analytical performances with detection limits reaching 0.0014 µg g?1 for As, 0.0016 µg g?1 for Cd, 0.012 µg g?1 for Cr, 0.0035 µg g?1 for Hg, 0.0055 µg g?1 for Mn, 0.10 µg g?1 for Ni, 0.0012 µg g?1 for Sb, 0.0083 µg g?1 for Sn, 0.011 µg g?1 for Se and Pb. The accuracy of the method was tested on a human hair ERM® certified reference material. Percent recoveries varied from 91.3% and 106.9% being always in the acceptance range of 90–110%. For all analysed elements, RSD% of repeatability ranged between 0.6% and 9.0% and those of intermediate precision did not exceed the limit of 20% being always lower than 10% (except for As). The proposed method was applied for the determination of trace elements in hair samples from 20 unexposed subjects. The geometric mean levels were as follows: Cr 0.28 µg g?1, Mn 0.30 µg g?1, Sn 1.04µg g?1, Sb 0.07 µg g?1, Hg 0.42 µg g?1, As 0.02 µg g?1, Cd 0.03 µg g?1, Ni 0.51 µg g?1, Se 0.45 µg g?1 and Pb 1.83 µg g?1. Element concentrations were in the same range with the reported data. The reported results may be useful for environmental exposure assessment or comparisons studies when establishing reference values of trace elements in exposed population.  相似文献   

14.
Nil Ozbek 《Analytical letters》2017,50(13):2139-2146
Elemental analysis of tarhana, a traditional Turkish cereal soup, has been conducted. A new method was developed for the determination of calcium, iron, magnesium, manganese, potassium, and sodium, in tarhana by microwave induced plasma atomic emission spectrometry. A sample of 0.1?g were mineralized by microwave digestion in 10?mL of 65% HNO3. A wheat flour standard reference material (GBW 08503) was used for validation. Linear calibration using standards prepared in acid was conducted for all determinations. The limits of detection were 1.21?µg?g?1 for Ca at 393.366?nm, 0.43?µg?g?1 for Fe at 259.940?nm, 11.5?µg?g?1 for K at 766.491?nm, 0.12?µg?g?1 for Mg at 285.213?nm, 0.04?µg?g?1 for Mn at 403.076?nm, and 0.04?µg?g?1 for Na at 588.995?nm. Ca, K, Fe, Mg, Mn, and Na were determined in tarhana with values from 0.73 to 1.61, 0.016 to 0.061, 2.02 to 4.09, 0.473 to 1.414, 0.019 to 0.043, and 0.26 to 1.83?mg?g?1, respectively.  相似文献   

15.
A reliable method was proposed for the simultaneous determination of five fluoroquinolones (FQs) and two tetracyclines (TCs) in sewage sludge using ultrasonic-assisted extraction (USE) followed by SPE cleanup and high-performance liquid chromatography-mass spectrometry (HPLC-MS)/MS analysis with electrospray ionisation (ESI) in a positive mode. The USE conditions (e.g. extraction solvent, pH, and extraction cycles) and high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) parameters were optimised. Quantification was performed by internal standard calibration in multiple reaction monitoring mode. Recoveries of the antibacterials ranged from 41 to 123%, with relative standard deviations within 17%. The sample-based limits of quantification were 10–63?ng?g?1 dry weight (dw) for FQs (ciprofloxacin, enrofloxacin, lomefloxacin, norfloxacin, and ofloxacin) and 250–500?ng?g?1 dw for TCs (tetracycline and oxytetracycline). The method was applied to determine the antibacterials in sewage sludge and sediment samples were collected from the Pearl River Delta, China. Ciprofloxacin, norfloxacin, and ofloxacin were frequently detected, ranging from 1052 to 17740?ng?g?1 dw in dewatered sludge samples, 585–3545?ng?g?1 dw in untreated solids, and 98–258?ng?g?1 dw in an urban stream sediment sample, respectively. Lomefloxacin and enrofloxacin were also occasionally detected.  相似文献   

16.
A simple and rapid method of ionic liquid based dispersive liquid-liquid microextraction(DLLME) combining with high performance liquid chromatography(HPLC) was developed for the analysis of four toxic anilines in flour steamed bread and maize steamed bread.Several possible influential factors such as the type of ionic liquid and disperser solvent,extraction time,sample pH,ionic strength and the volume of ionic liquid and disperser solvent were optimized using single factor experiments and orthogonal array design(OAD) with OA 25(5 4) matrix.Analysis of variance(ANOVA) and percent contribution(PC) were used to investigate the significance of the factors of OAD.Sample pH and ionic strength are statistically demonstrated two chief factors.Under the optimum condition,the method exhibits a good linearity(r 2 > 0.99) over the studied range(50-1000 ng g 1) for anilines.The extraction factors and recoveries for the anilines in two kinds of steamed breads ranged between 34.1%-73.3% and 44.3%-95.3%,respectively.The limit of detections(LODs) and limit of quantitations(LOQs) ranged between 10-15 ng g 1 and 30-45 ng g-1.  相似文献   

17.
129I is important as an environmental tracer of the biogeochemical cycling of iodine and of the dissemination of nuclear pollution, because anthropogenic 129I has been released from only few point sources and with its short mixing time its distribution therefore reveals the movement of 129I in the environment. A radiochemical neutron activation analysis method was developed to measure the concentration of 129I in soil samples. A procedure to pre-concentrate iodine from up to 150?g of soil was developed and validated using IAEA standard reference material IAEA-375 (Chernobyl soil). The method was applied to determine 129I/127I isotopic ratios as well as 129I and 127I concentrations in soils from several locations in Ukraine collected in 2006, 1996, 1993 and 1989, and from Slovenia, collected at various places in 2009 and 2006. The 127I concentrations in surface soils from Ukraine were in the range 2.3–23.1?µg?g?1 and for 129I (11.1–245.7)?·?10?8?µg?g?1 dry matter with the highest value of 1.47?·?10?3?µg?g?1 found in a soil sample collected in Yaniv, Ukraine in July 1993. In soil samples from Slovenia 127I concentrations ranged 0.73–130?µg?g?1 and 129I (8.0–245.7)?·?10?8?µg?g?1. The 129I/127I isotopic ratios of surface soils from Ukraine were in the range of the order of 10?9–10?5 and of 10?10–10?8 for soils from Slovenia. The highest isotopic ratio 13.6?·?10?5 was found in a soil sample collected in Yaniv, Ukraine in July 1993.  相似文献   

18.
A single robust reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated as per International Conference on Harmonization guidelines for the accurate quantification of curcuminoids in commercial turmeric products, Ayurvedic medicines, and nanovesicular systems. The proposed chromatographic method was found to be specific, linear (r2?≥?0.999), precise at intra- and inter-day levels (percentage relative standard deviation <2.0%), accurate (percentage recovery 99.14–102.29%), and robust. The limits of detection and quantification were found to be 7.40 and 24.70?ng?mL?1 for curcumin, 9.24 and 30.80?ng?mL?1 for demethoxycurcumin, and 6.48 and 21.61?ng?mL?1 for bisdemethoxycurcumin, respectively. Among different commercial turmeric products and Ayurvedic medicines tested, the contents of curcumin (3.54?±?0.06–25.8?±?0.08?mg?g?1), demethoxycurcumin (1.28?±?0.02–9.97?±?0.03?mg?g?1), and bisdemethoxycurcumin (0.50?±?0.01–5.97?±?0.01?mg?g?1) varied significantly. The developed method was effectively applied to the determination of encapsulation efficiency of curcuminoids (ranged between 84.33?±?3.50 and 96.59?±?2.53%) in the nanovesicular systems. In conclusion, the reported method is suitable for the analysis of curcuminoids in a wide variety of turmeric products and used for the quality control of products that contain curcuminoids.  相似文献   

19.
Selenium (Se) is a trace element essential to the well-being and health quality of humankind. Plant-derived foodstuffs, namely cereals, are the major dietary sources of Se in most countries throughout the world, even if Se contents are strongly dependent upon the corresponding levels in cereal-growing soils. Therefore, wheat is one of the staple crops that appears as an obvious candidate for Se biofortification, considering its gross-tonnage production and nutritional relevance worldwide. The present paper focuses on the ability of bread and durum wheat—Triticum aestivum L. and Triticum durum Desf., respectively—to accumulate Se after supplementation via a foliar-addition procedure. Two of the most representative wheat cultivars in Portugal—Jordão (bread) and Marialva (durum)—have been selected for supplementation trials, following the same agronomic practices and field schedules as the regular (non-supplemented) crops of those varieties (sowing: November 2010; harvesting: July 2011). Foliar additions were performed at the booting and grain-filling stages, using sodium selenate and sodium selenite solutions at three different Se concentrations—equivalent to field supplementation rates of 4, 20 and 100 g of Se per ha—with and without potassium iodide. Selenium contents in wheat grains obtained under foliar application are compared to data from regular wheat samples (field blanks) grown at the same soil/season, yet devoid of any Se supplementation. Total Se in all field samples was determined by cyclic neutron activation analysis (CNAA), via the short-lived nuclide 77mSe (half-life time: 17.5 s), in the Portuguese Research Reactor (RPI; CTN-IST, Sacavém). Quality control of the analytical procedure was asserted through concurrent analyses of NIST-SRM® 1567a (Wheat Flour). Results show that foliar additions can increase Se contents in mature grains up to 15 and 40 times for Marialva and Jordão, respectively, when compared to non-supplemented crops. Jordão and Marialva varieties responded differently to the stage of application.  相似文献   

20.
Ten yeast strains were evaluated concerning their capabilities to assimilate biodiesel-derived glycerol in batch cultivation. The influence of glycerol concentration, temperature, pH and yeast extract concentration on biomass production was studied for the yeast selected. Further, the effect of agitation on glycerol utilization by the yeast Hansenula anomala was also studied. The yeast H. anomala CCT 2648 showed the highest biomass yield (0.30?g?g?1) and productivity (0.19?g?L?1?h?1). Citric acid, succinic acid, acetic acid and ethanol were found as the main metabolites produced. The increase of yeast extract concentration from 1 to 3?g?L?1 resulted in high biomass production. The highest biomass concentration (21?g?L?1), yield (0.45?g?g?1) and productivity (0.31?g?L?1?h?1), as well as ribonucleotide production (13.13?mg?g?1), were observed at 700?rpm and 0.5?vvm. These results demonstrated that glycerol from biodiesel production process showed to be a feasible substrate for producing biomass and ribonucleotides by yeast species.  相似文献   

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