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1.
The potential of a prototype grazing-emission X-ray fluorescence spectrometer for reliable analysis of sample solutions, obtained by pressurized microwave oven digestion of Si-spiked organic and biological materials, was investigated as part of an inter-laboratory study. The fact that this grazing-emission technique is based on the total reflection phenomenon and wavelength-dispersive detection, gives it the benefit to determine light elements in a sensitive way. Results of the determination of silicon in pork liver, cellulose, urine, serum, spinach, beer, mineral water and horsetail (dry plant extract) samples are presented. Some of the results are compared with those obtained with other analytical techniques. The study proved that determination of silicon traces in biological matrices represents an extremely difficult task, however, measurements of silicon are achieved with acceptable precision. The most important problems still arise when sample pre-treatment is needed prior to analysis.  相似文献   

2.
We aimed to investigate the pharmacokinetics, bioavailability and urinary excretion of scopolin and its metabolite scopoletin in rats. An LC–tandem mass spectrometry (MS/MS) method for simultaneous determination of scopolin and scopoletin in rat biomatrices was developed and validated over a plasma and urine concentration range of 5.0–2000 ng/mL. Chromatographic separation was performed on a Hypersil GOLD C18 column with acetonitrile and 0.1% formic acid in water as mobile phase with gradient elution. Detection was performed in the positive ionization and selected reaction monitoring mode. The intra‐ and inter‐batch precision and accuracy, extraction recovery and matrix effect and stability of scopolin and scopoletin were well within the acceptable limits of variation. There was no gender‐related difference in the pharmacokinetic profiles of scopolin. There were significant differences in total area under the concentration–time curve (AUC), time required to achieve a maximal concentration (Tmax) and apparent clearance from plasma (Cl/F) of scopoletin between the male and female rats (p < .05). The bioavailability (F) of scopolin was exceptionally low. The maximal excretion rates were 7.61 μg/h and 7.15 μg/h for scopolin and 31.68 μg/h and 25.58 μg/h for scopoletin in male and female rats, respectively. The LC–MS/MS method was successfully applied to the pharmacokinetic, bioavailability and urinary excretion studies of scopolin and its metabolite scopoletin following a single administration of scopolin to rats.  相似文献   

3.
In this work three methods to diminish the content of most highly abundant proteins in human serum have been studied and compared. Protein depletion with ACN or DTT and protein equalization with the ProteoMiner? (PM) have been assessed by 1‐D gel electrophoresis and MS. After treatment 5, 18 and 9 major proteins within the 20 most abundant proteins in serum were identified for the ACN, DTT and PM methods, respectively. The ACN method was efficient for depleting high molecular weight proteins, over 75 KDa, resulting in 10±4% (n=3) of the total protein content remaining in the depleted serum. In addition, 75% of the proteins belonging to the group of the 20 most abundant proteins were not detected, making this depletion strategy a cheap alternative to expensive commercial tools regularly used for removing high abundance proteins from serum. The ACN extract was found rich in apolipoproteins. The dithithreitol method promotes the precipitation of proteins rich in disulfide bonds, mainly albumin, with 73±7% (n=3) of the total protein content remaining in the depleted serum, which was found rich in immunoglobulins. The PM method compresses the dynamic range of the serum proteins, rendering an extract containing 16±2% (n=3) of the total initial protein content. The extract was found to be rich in both apolipoproteins and immunoglobulins. As a general rule the DTT and PM methods provide a compression of the dynamic range of serum protein concentrations while the ACN method allows an effective depletion of the protein fraction above 72 KDa.  相似文献   

4.
New research has indicated that Gastrodiae Rhizome (GR) has potential anti‐diabetic and anti‐asthmatic effects in mouse models. On the basis of our previous study of the relative bioavailability of gastrodin (GAS) and parishin (PA) from extract and powder of GR, we performed further research on the tissue distribution and excretion of the two analytes. A reliable bioanalytical method for the quantification of GAS and PA in rat tissues and excretion is required. Chromatographic separation was carried out on a gradient mobile phase of acetonitrile–water with 0.1% formic acid. Calibration curves (1/x 2 weighted) offered satisfactory linearity (r 2 > 0.9835) within 100–3000 ng mL−1 for GAS and (r 2 > 0.9862) within 10–1000 ng mL−1 for PA. The relative standard deviations of the intra‐day and inter‐day precision were all <14.98%, whilst the relative errors of the intra‐day and inter‐day accuracy were all within ±14.71%. The matrix effect and recovery values were satisfactory in all of the biological matrices examination. The data of relative differences in tissue distribution and excretion of GAS and PA from powder and extract of GR indicated that higher bioavailabilities for GAS and PA were obtained when a dosage of 4 g kg−1 GR powder was used.  相似文献   

5.
An immunochemical assay was developed for the detection of metabolites excreted in urine as a result of occupational exposure to PAHs and nitro-PAHs. These metabolites were analyzed in a competitive ELISA, using an existing antibody (4D5) that has been developed against 6-aminobenzo[a]pyrene coupled to bovine serum albumine (B[a]P-BSA). A solid phase extraction (SPE) work-up procedure was optimized by dilution of pooled urine samples from rats exposed to 1-NP, in human urine. The application was validated by comparison of test results with urinary excreted 1-hydroxypyrene (1-OH-P) levels in a study among 28 railroad workers. Excretion of urinary metabolites was determined over two consecutive workdays. The 24 h average excretion of metabolites as determined in the immunoassay was not related to levels of particulate matter in the breathing zones of workers, not to 1-OH-P excretion levels of the day of urine collection. However, it was significantly associated with the personal dust exposure of the day before (P<0.0001), suggesting slow excretion of urinary metabolites. Smoking habits caused minor interference (P<0.1).  相似文献   

6.
Ion chromatography coupled with mass spectrometry is an established technique for determination of ionic analytes, however, sophisticated buffer removal equipment is required to eliminate inorganic compounds from the eluate before introduction into the ion source of mass spectrometer. A standard high‐performance liquid chromatography coupled with tandem mass spectrometry setup using an ion exchange column (Metrosep® A Supp 5) is proposed as an alternative approach. For that reason, some buffers including non‐volatile carboxylic acid based solutions have been evaluated for simultaneous trace determination of ionic and acidic pesticides including glyphosate in the same extract without a need for sophisticated buffer removal equipment. Two differently designed ionisation sources were compared qualitatively for the application of non‐volatile buffers. The study revealed that the choice of buffers had a strong influence on matrix effects in case of spiked extract injections. Finally, pesticides with very different physicochemical properties (logP < 0, logP ≥ 0) and structures (containing carboxylate, phosphonate, azolide, azanide, phenolate, bromate, and chlorate moieties) were quantified in spiked beer and oat extracts with acceptable recoveries (80–110%) using tandem mass spectrometry detection with AB SCIEX QTRAP 5500 instrument after separation using edetate buffer.  相似文献   

7.
Aristotelia chilensis is a plant rich in phenolics and other bioactive compounds. Their leaves are discarded as waste in the maqui berry industry. A new application of these wastes is intended by the recovery of bioactive compounds using pressurized hot water extraction with conventional or microwave heating. Both technologies have been selected for their green character regarding the type of solvent and the high efficiency in shorter operation times. Extractions were performed in the temperature range 140–200 °C with a solid/liquid ratio of 1:15 (w:w). The extracts’ total phenolic content, antioxidant capacity, and saccharides content obtained with both heating methods were measured. Additionally, the thermo-rheological properties of the gelling matrix enriched with these extracts were analyzed. Optimum conditions for lyophilized extracts were found with conventional heating, at 140 °C and 20 min extraction; 250.0 mg GAE/g dry extract and 1321.5 mg Trolox/g dry extract. Close to optimum performance was achieved with microwave heating in a fraction of the time (5 min) at 160 °C (extraction), yielding extracts with 231.9 mg GAE/g dry extract of total phenolics and antiradical capacity equivalent to 1176.3 mg Trolox/g dry extract. Slightly higher antioxidant values were identified for spray-dried extracts (between 5% for phenolic content and 2.5% for antioxidant capacity). The extracts obtained with both heating methods at 200 °C contained more than 20% oligosaccharides, primarily glucose. All the formulated gelling matrices enriched with the obtained extracts displayed intermediate gel strength properties. The tested technologies efficiently recovered highly active antioxidant extracts, rich in polyphenolics, and valuable for formulating gelling matrices with potential applicability in foods and other products.  相似文献   

8.
This study examined the efficacy of hydroalcoholic extract of dried clove buds, which is rich in phenolic compounds namely eugenol and eugenol derivatives (precursors of flavones, isoflavones and flavonoids), on different primary and secondary osteoporotic marker changes in an ovariectomised (OVX) rat model of osteoporosis. Female Wistar rats were randomly divided into three groups: sham-operated control (A), OVX (B) and OVX plus 50% hydroalcoholic extract of dried clove buds for 4 weeks (C). Results indicated that, compared to control, serum alkaline phosphatase (AP; 48.25%, p?相似文献   

9.
Summary The cadmium excretion was determined in urine samples obtained from 270 inhabitants of a cadmiumpolluted quarter of Stadskanaal and from 282 persons of a control group.The urinary cadmium concentration was determined by using atomic-absorption spectroscopy with electrothermal atomization. Quantitation was performed by a standardaddition technique. The detection limit was 0.05 g Cd/l. The working range was linear from 0.05 to 3.5g Cd/l. The coefficient of variation of duplicate measurements was 1–5%. The squared average coefficient of variation obtained from 23 samples analyzed in duplicate was 9.5%.The influence of some factors (smoking habits and sex), which were expected to increase the urinary cadmium excretion, was studied in the control group. Compared to the reference level of non-smoking male controls the cadmium excretion was significantly higher in non-smoking female controls (P< 0.001) and in smoking male controls (P< 0.001). Compared to the non-smoking female controls smoking increased the cadmium excretion of smoking female controls significantly (0.01 <P< 0.05).The cadmium exposure of the inhabitants was evaluated on the basis of their urinary cadmium excretion compared to the control group. With respect to the corresponding control groups the urinary cadmium excretion of the inhabitants was only just significantly higher in the category of non-smoking males (P = 0.05).
Bestimmung der Cadmiumausscheidung im Harn zur Beurteilung der Cd-Exposition von Bewohnern eines Cd-belasteten Stadtteiles von Stadskanaal
Zusammenfassung Die Cadmiumausscheidung wurde in Harnproben von 270 Einwohnern eines Cd-belasteten Stadtteiles von Stadskanaal sowie von 282 Teilnehmern einer Kontrollgruppe bestimmt.Als Bestimmungsverfahren diente die Atomabsorptionsspektroskopie mit elektrothermischer Atomisierung. Die quantitative Auswertung erfolgte nach der Standard-Zugabe-Methode. Die Nachweisgrenze lag bei 0,05 g Cd/l. Der Arbeitsbereich war linear von 0,05 bis 3,5 g Cd/l. Der Variationskoeffizient von Doppelmessungen betrug 1–5%. Der quadratische Durchschnitt der Variationskoeffizienten von 23 Proben ergab sich zu 9,5%.Bei der Kontrollgruppe wurde der Einfluß einiger Faktoren (Rauchgewohnheiten und Geschlecht) untersucht, die zur Erhöhung der Cadmiumausscheidung beitragen. Im Vergleich zu den männlichen Nichtrauchern der Kontrollgruppe war die Cd-Ausscheidung bei den weiblichen Nichtrauchern (P< 0,001) und den männlichen Rauchern derselben Gruppe signifikant höher (P< 0,001). Im Vergleich zu den weiblichen Nichtrauchern der Kontrollgruppe wurde die Cd-Ausscheidung durch Rauchen bei dieser Gruppe deutlich erhöht (0,01 <P< 0,05).Die Cadmiumexposition der Bewohner wurde aufgrund ihrer Cd-Ausscheidung im Vergleich zu der Kontrollgruppe bewertet. In bezug auf die entsprechenden Kontrollgruppen war die Cd-Ausscheidung der Bewohner nur bei den männlichen Nichtrauchern gerade signifikant größer (P = 0,05).


Dedicated to Prof. Dr. W. Fresenius on the occasion of his 70th birthday  相似文献   

10.
Fenugreek is used as a spice and a traditional herbal medicine for a variety of purposes, given its antidiabetic and antioxidant effects. Self-emulsifying drug delivery systems (SEDDS) of herbal drugs are targets of extensive research aiming to increase bioavailability and stability. The study’s objective was to formulate SEDDS containing Trigonella foenum-graecum extract to improve the stability of herbal extract and to increase their permeability through a Caco-2 monolayer. A characterized fenugreek dry extract was used for the formulations, while the SEDDS properties were examined by particle size analysis and zeta potential measurements. Permeability assays were carried out on Caco-2 cell monolayers, the integrity of which was monitored by follow-up trans-epithelial electric resistance measurements (TEER). Cytocompatibility was tested by the MTT method, and an indirect dissolution test was performed, using DPPH antioxidant reagent. Two different SEDDS compositions were formulated from a standardized fenugreek dry extract at either the micro- or the nanoemulsion scale with sufficient stability, enhanced bioavailability of the compounds, and sustained release from HPMC capsules. Based on our results, a modern, non-toxic, cytocompatible fenugreek SEDDS formulation with high antioxidant capacity was developed in order to improve the permeability and bioavailability of all components.  相似文献   

11.
Study evaluates testis mass in rats subjected to early weaning and subsequently nourished with diet containing flour or flaxseed oil. Pups were weaned for separation from mothers at 14 days (early weaning, EW) and 21 days (control, C). After 21 days, the control group (C60) was nourished with control diet. EW was divided as: control (EWC60), flaxseed flour (EWFF60) and flaxseed oil (EWFO60) group diets for the next 60 days. At 21st and 60th day, body mass, serum cholesterol and triglycerides and testis mass were evaluated. At 21 day, EW group showed lower (p < 0.05) body mass, serum cholesterol and testis mass. At 60 days, EWC60 and EWFO60 groups showed lower (p < 0.05) body mass (vs. C60 and EWFF60). EWFF60 group showed lower (p < 0.05) serum cholesterol (vs. EWC60 and EWFO60) and higher (p < 0.05) testis mass (vs. C60, EWC60 and EWFO60). Flaxseed flour (vs. oil) was associated with higher testis mass following early weaning.  相似文献   

12.
In an extract of spore-bearing stems ofEquisetum arvense L. (field horsetail) saponaretin, apigenin 5-glucoside, luteolin 5-glucoside, kaempferol 3-sophoroside, quercetin 3-glucoside, 4-hydroxy-6-(2-hydroxyethyl)-2,2,5,7-tetramethylindanone, and a compound of ketonic nature, isolated previously from an extract of the herbage of the field horsetail, have been identified by high-performance liquid chromatography. The characteristics of the chromatographic behavior of glycosylated flavones under the conditions of reversed-phase liquid chromatography have been studied and it has been shown that the glycosylation of flavones at position 5 of the molecule causes a greater fall in the affinity for a nonpolar stationary phase than in position 7 of the molecule.Irkutsk Institute of Organic Chemistry, Siberian Branch of the Academy of Sciences of the USSR. First I. M. Sechenov Moscow Medical Institute. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 334–337, May–June, 1980.  相似文献   

13.
Retrorsine (RTS) is a toxic retronecine-type pyrrolizidine alkaloid, which is widely distributed. The purpose of this study was to develop a high-performance liquid chromatography–tandem mass spectrometric (LC–MS/MS) method for serum RTS determination in mice. Serum samples were deproteinated by acetonitrile, separated on a C18-PFP column and delivered at 0.8 ml/min with an eluting system composed of water containing 0.1% (v/v) formic acid and acetonitrile containing 0.1% (v/v) formic acid as mobile phases. RTS and the internal standard S-hexylglutathione (H-GSH) were quantitatively monitored with precursor-to-product transitions of m/z 352.1 → 120.1 and m/z 392.2 → 246.3, respectively. The method showed excellent linearity over the concentration range 0.05–50 μg/ml, with correlation coefficient r2 = 0.9992. The extraction recovery was >86.34%, and the matrix effect was not significant. Inter- and intra-day precisions (RSD) were <4.99%. The validated LC–MS/MS method was successfully applied to study the toxicokinetic profiles of serum RTS in mice after intravenous, oral administration and co-treated with ketoconazole, which showed that RTS displayed a long half-life (~11.05 h) and good bioavailability (81.80%). Co-administration of ketoconazole (KTZ) increased the peak serum concentration and area under the concentration–time curve and decreased the clearance and mean residence time. Summing up, a new standardized method was established for quantitative determination of RTS in sera.  相似文献   

14.
Chiral phenylethyl alkylammonium montmorillonites were prepared by ion exchange of Na montmorillonite (from Wyoming). The structure of chiral montmorillonite organocomplexes was studied in the dry state by X-ray diffraction, IR spectroscopy and 13C cross-polarized MAS NMR and after swelling by X-ray diffraction. The phenylethylammonium ions are intercalated in montmorillonite in a monolayer structure, while higher derivatives containing alkyl chains with lengths of n c=10−16 take up a bilayer orientation. The hydrophobized clay mineral is readily dispersed in organic solvents, for example in ethanol, toluene and their binary mixtures. Due to selective adsorption, the liquids penetrate into the interlamellar space under significant interlayer expansion producing a great variety of alkyl chain orientations within the interlamellar space, depending on the length of alkyl chains and on the mixture composition. Such interlamellar spaces are possible chiral nanoreactors with adjustable volume and may be prospectively utilized for shape-selective catalytic reactions and the production of enantiomers. Received: 20 July 1998 Accepted in revised form: 22 September 1998  相似文献   

15.
Proteins can be an excellent by product of the biorefining of lignocellulosic materials. In this work, extraction conditions for the white leaf proteins (cytoplasmic) of ammonia-treated dwarf elephant grass were established to obtain a protein juice suitable for the production of leaf protein concentrates. A calcium hydroxide solution was used as extracting agent, at several solid-liquid ratios, pHs, temperatures, and times. Extractions were carried out in Erlenmeyer flasks containing 5 g (dry basis) of forage with constant agitation (100 rpm). The soluble protein content was determined by the Lowry method. Optimal extraction conditions for the ammonia-treated forage were 12.60 pH, 1:10 solid-liquid ratio, 90°C, and 30 min extraction time, resulting in 52.65% extraction yield. The ammonia treatment significantly increased (p<0.05) the release of proteins from the fibrous matrix, facilitating their extraction.  相似文献   

16.
Water absorption in thin films (<1000 Å) of a commercial polyimide was evaluated by monitoring dimensional changes induced by a humid environment. Film thickness was measured using x-ray reflectivity, which is a nondestructive technique offering angstrom resolution in the measurements of thin film or multilayer thickness. The effect of several variables on the absorption of moisture were monitored in polyimide films adhered to polished silicon substrates, including total dry film thickness, exposure time, and the contribution of a coupling agent. The percentage increase in film thickness due to moisture uptake is found to be a weak function of dry film thickness, decreasing as dry film thickness increases, and to be somewhat affected by the use of an interfacial coupling agent. The observed behavior points to the polymer/substrate interface as a strong factor controlling the absorption of moisture in the polyimide/silicon system, and is believed to reflect the presence of a highly moisture-saturated interfacial layer. A bilayer model is proposed, and the feasibility of using this model to describe the observed behavior is considered. Published 1998 John Wiley & Sons, Inc.
  • 1 This article is a US Government work and, as such, is in the public domain in the United States of America.
  • J Polym Sci B: Polym Phys 36 : 155–162, 1998  相似文献   

    17.
    In order to gain further insight into the protective action of Na2MoO4 pretreatment (1.24 mmol/kg, once a day, i.p.) against the acute toxicity of HgCl2 (30 mummol/mmol/kg, once, s.c.), changes of renal function, tissue accumulation of mercury, and urinary excretions of mercury and phenolsulfonphthalein after exposure to HgCl2 were investigated. Lactate content in the kidney and serum calcium were also measured. Na2MoO4 pretreatment enhanced urinary excretion of mercury. Renal function of Na2MoO4-pretreated rats was better maintained as compared to that of the rats given HgCl2 alone at either dose (30 or 15 mumol/kg) although the metal content in the kidney of this group was almost the same as that of the latter HgCl2-alone rats. This pretreatment prevented the rise in lactate content in the kidney and the reduction of urinary excretion of phenolsulfonphthalein caused by HgCl2, Na2MoO4 reduced serum calcium. These results suggest that Na2MoO4 prevented mercury-induced acute renal failure by decreasing tissue accumulation of the metal through urinary excretion of mercury. Better renal hemodynamics attributable to hypocalcemia may be a causative factor in the enhancement of urinary excretion of mercury.  相似文献   

    18.
    By using the adsorbent Saccharomyces cerevisiae immobilized on sepiolite an adsorption-elution method was developed for the preconcentration of Cu, Zn, and Cd followed by flame atomic absorption spectrometry (FAAS). Recoveries were 98.3 ± 0.4% for Cu, 94.2 ± 0.3% for Zn, and 99.04 ± 0.04% for Cd at 95% confidence level obtained by the column method. The influence of sea water matrix elements on the separation of the trace elements was also assessed by using the column procedure. The breakthrough capacities were found to be 74 μmol/g for copper, 128 μmol/g for zinc and 97 μmol/g for cadmium. After optimization the proposed method was applied to the trace metal determination in sea and river water. Received: 8 June 1998 / Revised: 8 September 1998 / Accepted: 16 September 1998  相似文献   

    19.
     A series of P[N-isopropylacrylamide (NIPAM)] latexes with different contents of cyano groups were successfully prepared by either seeded or shot-growth polymerizations of an aqueous solution containing acrylonitrile (AN) onto a seed P[NIPAM] latex, respectively, and further characterized by FT-IR, 1H-NMR, elemental analysis, as well as by quasielastic light scattering (QELS) and scanning electron microscopy (SEM). All prepared surface-cyanofunctionalized P[NIPAM] latexes exhibited the same range of lower critical solution temperature (LCST) as a pure P[NIPAM] latex. The shot polymerization process proved more efficient at yielding cyano derivatized latexes than the seeded polymerization technique. The amount of incorporated cyano groups onto the particles was determined with a good correlation both by 1H-NMR and elemental analysis. The higher the amount of initially introduced AN monomer in the reaction mixture, the more cyano groups were incorporated onto the particles. The surface of the particles with high content of cyano groups appeared quite rough by SEM in comparison with that of the pure P[NIPAM] particles. Received: 25 February 1998 Accepted: 23 June 1998  相似文献   

    20.
    Summary NIST issues food related, chemical composition standard reference materials for validating food analyses. SRMs certified for inorganic constituents are: Non-Fat Milk Powder (SRM 1549), Oyster Tissue (SRM 1566a), Bovine Liver (SRM 1577a), Wheat Flour (SRM 1567a), Rice Flour (SRM 1568a), and Total Diet (SRM 1548). The certificate of analysis for the total diet SRM also provides a certified concentration for cholesterol. Oyster tissue, a renewal SRM, is certified for 25 elements including 6 (Al, Cl, I, P, S, and V), that had not been certified in the previously issued SRM 1566. The elemental certified concentrations are based on concordant results of two or more independent analytical methods. The chemical compositions of the six food matrix SRMs are tabulated. Three food matrix SRMs certified for organic constituents are: Cholesterol and Fat-Soluble Vitamins in Coconut Oil (SRM 1563), Cholesterol in Whole Egg Powder (SRM 1845) and Organics in Cod Liver Oil (SRM 1588). Serum and urine matrix SRMs are also available that may be useful for metabolic and bioavailability studies.  相似文献   

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