首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
In this study, human meniscus tissue of normal origin in young adults and in patients with early and late stages of osteoarthritic degeneration were analyzed for their thermoanalytical properties with differential scanning calorimetry. Degenerative changes of knee menisci frequently result from trauma to the joint or are associated with joint diseases. Meniscus damage may play an important role in osteoarthritis pathophysiology. The purpose was to further characterize the altered metabolism in matrix composition during different stages of meniscus degeneration that promotes disease progression. The human knee joint menisectomy specimens were received after surgical removal. The calorimetric properties of samples were determined by DSC method, samples were heated from 0 to 80 °C. The heating rate was 0.3 °C min?1. Conventional Hastelloy batch vessels were used with 40 μL sample volume. Change in the enthalpy was observed in normal cartilage as 1632.48 J g?1 (SD = 50.55). In case of early degeneration a greater change at 1707.83 J g?1 (SD = 112.46), while in the severely degenerated samples at 1677.30 J g?1 (SD = 182.48) was measured. This method proved to be suitable for compositional thermoanalytical study of normal and degenerative human meniscus samples. All samples that were extracted for this study were obtained during live surgeries. With the rise of temperature an endothermic reaction was observed in all cases. The enthalpy change of the process initiated by the temperature change showed difference between the normal and pathological groups.  相似文献   

2.
The Dupuytren contracture - degenerative shortening of the palmar aponeurosis - is a common disease of the hand in Europe. The aetiology of the degenerative changes in the collagen structures is still not clear. To describe the clinical manifestation of the disease we use an international classification according to Iselin. Our hypothesis was that in Dupuytren disease there is a clear pathological abnormality in the tissue elements building up the palmar aponeurosis, which is responsible for the disease, and could be monitored besides the classical histological methods by differential scanning calorimetry. The thermal denaturation of different parts of human samples was monitored by a SETARAM Micro DSC-II calorimeter. All the experiments were performed between 0 and 100°C. The heating rate was 0.3 K min−1. DSC scans clearly demonstrated significant differences between the different types and conditions of samples (control: T m=63°C and ΔH cal=4.1 J g−1, stage I.: T m= 63°C and ΔH cal=5.1 J g−1, stage II.: T m=64°C and ΔH cal=5.2 J g−1, stage III.: T m=60°C and ΔH cal=5.2 J g−1, stage IV.: T m=60.2°C and ΔH cal=5.3 J g−1). The heat capacity change between native and denatured states of aponeurosis samples increased with the degree of structural alterations indicating significant water loosing. These observations could be explained with the structural alterations caused by the biochemical processes. With our investigations we could demonstrate that DSC is a useful and well applicable method for the investigation of collagen tissue of the human aponeurosis. Our results may be of clinical relevance in the future i.e. in the choice of the optimal time of surgical therapy of different clinical level Dupuytren contractures.  相似文献   

3.
Osteonecrosis (ON) of the femoral frequently occurs after steroid medication. One of the final pathways leading to steroid induced ON is thought to be pathologic fat metabolism. The pathobiological mechanism underlying the induction of fat metabolism outslides by steroids leading to ON has not been fully elucidated. The purpose of this study was to examine the intraoperative obtained gluteal fat tissue from ON patients with histology, gas chromatography (GC) and differential scanning calorimetry (DSC) and to compare them with otherwise healthy patient’s samples. The histological sections showed no significant differences compared with the control group. GC revealed that fraction of saturated fatty acids decreased in ON samples from mean values of controls of 24% to 21, the polyunsaturated fraction from 20 to 14%. The monounsaturated acids showed an increase from mean rate of 52% of the controls to 65% of steroid treated samples. DSC curves correlate with chromatographic analysis of the tissue fatty acids (Steroid treated, heating between 0–100°C: T m=5.7°C, ΔH= −15.8J/g−1; heating between −20–100°C: Tm= −9.96 and 5.85°C, ΔH= −59.17 and −16.2 J g−1. Non-necrotic, heating between 0–100°C: two separable transition with Tm=5.7 and 9.9°C, total ΔH= −20.8 J g−1; heating between −20–100°C: Tm= −10.9 and 4.95°C, total ΔH= −75.8 J g−1.) Our preliminary findings are rather tendentious. Further investigations are needed with higher sample rate and under other anamnestic circumstances too.  相似文献   

4.
The World Health Organization states that envenomation is responsible for a high number of deaths per year, especially in equatorial areas. The only effective specific treatment is the use of hyperimmune serum (antivenom). In Brazil, Crioula breed horses are used for antivenom production, with great importance in the maintenance of public health programs. A strict biochemical and metabolic control is required to attain specificity in antiserum. Inorganic elements represent only a small fraction of whole blood. Nonetheless, they play important roles in mammalian metabolism, being responsible for controlling enzymatic reactions, respiratory and cardiac functions and ageing. In this work, whole blood samples from Crioula breed horses were analyzed by EDXRF technique. The reference interval values were determined for the elements Na (1955–2013 μg g−1), Mg (51–75 μg g−1), P (523–555 μg g−1), S (1628–1730 μg g−1), Cl (2388–2574 μg g−1), K (1649–1852 μg g−1), Ca (202–213 μg g−1), Cu (4.1–4.5 μg g−1) and Zn (2.4–2.8 μg g−1) and a comparative study with NAA results was outlined. The samples were obtained from Instituto Butantan. Both techniques showed to be appropriate for whole blood sample analyses and offer a new perspective in Veterinary Medicine.  相似文献   

5.
The heat of transformation (Q ) of the chains in amorphous sulfur doped with selenium (0, 2, 4 and 6 at%Se) and phosphorous (0, 0.43, 0.86 and 1.28 at%P) was measured calorimetrically. All samples were remelted at temperature T f =443 K. The admixtures decrease the Q : at the measurement temperature 298 K the mean value of is equal to 37.6, 20.4 and 9.1 J g−1 for the samples S, S+6 at%Se and S+1.28 at%P respectively. The quantity of the evolved heat increases vs. the elevation of the measurement temperature. For the samples S+6 at%Se the value is equal 16.2 and 28.8 J g−1 at 288 to 303 K. For the samples S+1.28 at%P the value of increases from 9.1 to 25.0 J g−1 in the range of the measurement temperature from 293 to 308 K. The results are discussed on the basis of the theory of nucleation and growth of nuclei. This revised version was published online in August 2006 with corrections to the Cover Date.  相似文献   

6.
The applicability of fast and thermal neutron activation analyses for the determination of gold in rock samples has been studied. Using a Ge/Li/ detector limit of 0.45 mg g−1 was obtained for a fast neutron flux of 8.107 n cm−2.s−1. With a thermal neutron flux of 6.105 n cm−2.s−1 and the same detector a value of 35 μg g−1 was obtained. Using a NaI/Tl/ crystal a sensitivity of 14 μg g−1 was attained at the same thermal flux. This work was supported in part by the Hungarian Academy of Sciences.  相似文献   

7.
 Microwave digestion reduction-aeration and pyrolysis combined with cold vapour atomic absorption and cold vapour atomic fluorescence are compared for the determination of total mercury in several biological and environmental matrices. The biological samples were digested in a mixture of HNO3/H2O2, the environmental samples in a mixture of HNO3/HClO4. After reduction with SnCl2, the mercury was collected by two-stage gold amalgamation. After microwave digestion reduction-aeration, detection limits of 1.4 ng g−1 and 0.6 ng g−1 were obtained for cold vapour atomic absorption spectrometry (CVAAS) and cold vapour atomic fluorescence spectrometry (CVAFS), respectively, for 250 mg of environmental samples. For biological samples (500 mg) the detection limits were 0.7 ng g−1 (CVAAS) and 0.4 ng g−1 (CVAFS). After pyrolysis, detection limits of 3.5 ng g−1 and 1.6 ng g−1 for CVAAS and CVAFS, respectively, were obtained for a 10 mg sample. Pyrolysis can only be applied when the organic content of the sample is not too high. Accurate results were obtained for 8 certified reference materials of both environmental and biological origin. In addition, a real sludge sample was analysed. Author for correspondence. E-mail: richard.dams@rug.ac.be Received September 18, 2002; accepted December 3, 2002 Published online May 5, 2003  相似文献   

8.
Summary Nicotine has been analyzed by gas chromatography nitrogen-phosphorus detection in tissue samples obtained by repeated minimal trauma tissue biopsies from human subcutaneous adipose tissue. For sample preparation, a single extraction step of the tissue samples with chloroform was performed at 30–45°C. Calibration curves generated with spiked porcine subcutaneous adipose tissue were linear over a concentration range from 0.20 to 100 μg g−1, therefore, the limit of quantification was fixed at 0.20 μg g−1. The limit of detection was found to be 0.05 μg g−1 adipose tissue. The recovery of nicotinespiked porcine subcutaneous adipose tissue by chloroform extraction was 100±8%. The performance of the assay was not affected by the complex lipid matrix. The method was employed for analysis in a clinical study on nicotine penetration from a transdermal delivery system through the skin of moderate smokers. Presented at Balaton Symposium on High Performance Separation Methods, Siófok, Hungary, September 1–3, 1999.  相似文献   

9.
Summary A method for the determination of the food mutagen 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) in human hair has been developed and validated. Hair samples (200 mg) were dissolved in NaOH (1 M) and PhIP was isolated by successive solid-phase extraction on a polystyrene-divinylbenzene column and on a silica-based mixed-mode column with C8 and-SO3 functional groups. Quantification was performed by gas chromatography-electron-impact ionization high-resolution mass spectrometry in selected-ion-monitoring mode. The method was validated for determination of PhIP in the concentration range 0.5–25 ng g−1 hair with [2H3]PhIP as internal standard. The limit of quantification was 0.26 ng g−1 hair. Within-day and between-day precision were in the ranges 1–27% and 2–15% relative standard deviation, respectively. The hair sample used for method validation was found to contain 0.26 ng PhIP g−1 hair.  相似文献   

10.
A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation–atomic-fluorescence spectrometry (HG–AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L−1 H2SO4 and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g−1 for Sb(III), 1.0 ng g−1 for Sb(V), 1.3 ng g−1 for Se(IV), 1.0 ng g−1 for Se(VI), 1.1 ng g−1 for Te(IV), 0.5 ng g−1 for Te(VI), and 0.9 ng g−1 for Bi(III), in all cases expressed in terms of sample dry weight.  相似文献   

11.
The specific and non-specific interactions of twelve activated carbon cloth samples prepared from commercial cotton fabric, and that present different activation degrees are studied through the determination of immersion enthalpies in CCl4 and H2O, and in aqueous solutions of NaOH and HCl. The immersion enthalpies found for the solvents CCl4 and H2O are in a range of 5.49–45.84 and 1.77–7.76 J g−1, respectively. The enthalpic values for the materials in aqueous solutions of NaOH and HCl, allow characterizing the chemical surface of these materials, which are in a range of 6.63 and 21.49 J g−1, finding through them important relations in company with other characterizing techniques used in the study of these materials.  相似文献   

12.
A rapid method for the extraction and determination of 90Sr in natural water, plant and sediment samples was developed using extraction chromatography and dynamic reaction cell ICP–MS, with O2 as a reaction gas. While isobaric interference from the stable isotope 90Zr was efficiently removed by this method, interferences produced from in-cell reactions with Fe+ and Ni+ required suppression by tuneable bandpass, and in sediments, additional chromatographic separation. Method detection limits were 0.1 pg g−1 (0.5 Bq g−1), 0.04 pg g−1(0.2 Bq g−1), and 3 pg L−1 (5 Bq L−1) for sediments, plant and water samples, respectively, and 90Sr concentrations determined by ICP–MS were in good agreement with activities determined by Cerenkov counting and with certified reference values. While mass spectrometric determination does not rival detection limits achievable by radiometric counting, radiometric determination of 90Sr, a pure beta-emitter, is hindered by long analysis times (several weeks); the comparatively fast analysis achieved via ICP–MS enables same-day preparation and analysis of samples, making this an important technique for the environmental monitoring of areas contaminated by radioactivity.  相似文献   

13.
Summary Formaldehyde, as its dimedone adduct formaldemethone, has been detected and quantified in all the tested species of angiosperms, gymnosperms, pteridophytes, lichens and fungi, as well as in the two species tested of cyanobacteria and the one species of charophyte. Yields ranged from<10μg g−1 to 6940 μg g−1 fresh weight, calculated as formaldemethone (equivalent to <1 μg g−1 to 713 μg g−1 fresh weight, calculated as formaldehyde). An HPLC procedure was used for quantification of formaldemethone. A linear relationship was found between 20 and 2160 μg g−1 and the statistical limit of detection was calculated as 48 μg g−1.  相似文献   

14.
The objective of this research was to develop, optimize, and validate a modern, rapid method of preparation of human hair samples, using microwave irradiation, for analysis of eight tricyclic antidepressants (TCADs): nordoxepin, nortriptyline, imipramine, amitriptyline, doxepin, desipramine, clomipramine, and norclomipramine. It was based on simultaneous alkaline hair microwave-assisted hydrolysis and microwave-assisted extraction (MAH–MAE). Extracts were analyzed by high-performance liquid chromatography with diode-array detection (HPLC–DAD). A mixture of n-hexane and isoamyl alcohol (99:1, v/v) was used as extraction solvent and the process was performed at 60°C. Application of 1.0 mol L−1 NaOH and microwave irradiation for 40 min were found to be optimum for hair samples. Limits of detection ranged from 0.3 to 1.2 μg g−1 and LOQ from 0.9 to 4.0 μg g−1 for the different drugs. This enabled us to quantify them in hair samples within average therapeutic concentration ranges.  相似文献   

15.
An expeditious method for the determination of triclosan (TCS) and methyl triclosan (MTCS) in sludge and sediment samples is presented. Extraction and cleanup steps were integrated in the same process using matrix solid-phase dispersion as sample preparation technique. Effects of different variables on the efficiency and the selectivity of the sample preparation process are discussed. Under final working conditions, samples (0.5 g) were dispersed with diatomaceous earth (1 g) and transferred to a polypropylene syringe containing 2 g of silica impregnated with sulphuric acid (15%, w:w). Analytes were recovered with 10 mL of dichloromethane. After solvent exchange to ethyl acetate, TCS was converted into the tert-butyldimethylsilyl derivative, and the extract was analysed by gas chromatography-mass spectrometry, without any additional cleanup. Obtained recoveries, for sludge and sediment samples spiked at different concentration levels, ranged from 86% to 113%, with associated standard deviations between 2 and 13%. Limits of quantification of the global method were 6 and 7 ng g−1 for MTCS and TCS, respectively. Both compounds were detected in all the processed sludge samples with maximum concentrations of 191 ng g−1 (MTCS) and 2,640 ng g−1 (TCS). The parent bactericide was also found in some sediment samples at concentrations up to 200 ng g−1.  相似文献   

16.
The interactions among five samples of activated carbons, obtained from different lignocellulosic materials with different degrees of activation of approximately 20% and aqueous solutions of phenol and 4-nitro phenol are studied by means of the determination of immersion enthalpies. It is established that the obtained activated carbons are of a basic character and show values for the pH at the point of zero charge, pHPZC, that range from 7.4 to 9.7 and, in all cases, higher total basicity contents than the values obtained for total acidity. The immersion heat of the activated carbons in CCl4 and water is determined obtaining values which are higher for CCl4 immersion and vary from 31.4 to 48.6 J g−1. The hydrophobic factor, hf, it is calculated from the relation between of the immersion heat of the activated carbons in CCl4 and the immersion heat in water, the obtained values were 2.98 and 6.75, which are greater than 1 due to the greater values obtained in CCl4 when compared to the values obtained in water. Immersion enthalpies in phenol solution range from 7.6 to 13.9 J g−1 and for the case of 4-nitro phenol such enthalpies range from 12.7 to 20.5 J g−1; all the 5 samples studied showed a higher value for the heat of immersion in aqueous solutions of 4-nitro phenol.  相似文献   

17.
Research is needed to allow more efficient processing of lignocellulose from abundant plant biomass resources for production to fuel ethanol at lower costs. Potential dedicated feedstock species vary in degrees of recalcitrance to ethanol processing. The standard dilute acid hydrolysis pretreatment followed by simultaneous sacharification and fermentation (SSF) was performed on leaf and stem material from three grasses: giant reed (Arundo donax L.), napiergrass (Pennisetum purpureum Schumach.), and bermudagrass (Cynodon spp). In a separate study, napiergrass, and bermudagrass whole samples were pretreated with esterase and cellulose before fermentation. Conversion via SSF was greatest with two bermudagrass cultivars (140 and 122 mg g−1 of biomass) followed by leaves of two napiergrass genotypes (107 and 97 mg g−1) and two giant reed clones (109 and 85 mg g−1). Variability existed among bermudagrass cultivars for conversion to ethanol after esterase and cellulase treatments, with Tifton 85 (289 mg g) and Coastcross II (284 mg g−1) being superior to Coastal (247 mg g−1) and Tifton 44 (245 mg g−1). Results suggest that ethanol yields vary significantly for feedstocks by species and within species and that genetic breeding for improved feedstocks should be possible.  相似文献   

18.
Enrofloxacin is a synthetic bacteriostatic administered in veterinary therapy. It can also be used illegally as a growth promoter to enhance feed efficiency and weight gain. This practice is banned in several countries due to its potential negative effects on the environment and human health. A suitable method for extracting and quantifying enrofloxacin (ENR) and its main metabolite ciprofloxacin (CPR) in cattle and pig hair by high-performance liquid chromatography–fluorimetric detection (HPLC–FLD) had been proposed. ENR and CPR were extracted from hair samples with methanol acidified with trifluoroacetic acid for 24 h at 70 °C. The extracts were evaporated and redissolved in the mobile phase before injection. This simplified procedure enabled the detection of both CPR and ENR at ng g−1 levels (limit of detection 4–5 ng g−1) without further purification. Detectable residues of ENR were found in calf and pig hairs after the pharmacological treatment was started. Mean concentrations of quinolone (ENR, CPR) in contaminated hairs ranged from 20 to 2,518 ng g−1 in calves and from 152 to 1,140 ng g−1 in pigs. Hair pigmentation enhanced quinolone accumulation significantly. Hair analysis seems to increase the time window available for the retrospective detection of illegal ENR administration compared to edible tissue analysis.  相似文献   

19.
An accurate and sensitive multi-species species-specific isotope dilution GC–ICP–MS method was developed for the simultaneous determination of trimethyllead (Me3Pb+), monomethylmercury (MeHg+) and the three butyltin species Bu3Sn+, Bu2Sn2+, and BuSn3+ in biological samples. The method was validated by three biological reference materials (CRM 477, mussel tissue certified for butyltins; CRM 463, tuna fish certified for MeHg+; DORM 2, dogfish muscle certified for MeHg+). Under certain conditions, and with minor modifications of the sample pretreatment procedure, this method could also be transferred to environmental samples such as sediments, as demonstrated by analyzing sediment reference material BCR 646 (freshwater sediment, certified for butyltins). The detection limits of the multi-species GC–ICP–IDMS method for biological samples were 1.4 ng g−1 for MeHg+, 0.06 ng g−1 for Me3Pb+, 0.3 ng g−1 for BuSn3+ and Bu3Sn+, and 1.2 ng g−1 for Bu2Sn2+. Because of the high relevance of these heavy metal alkyl species to the quality assurance of seafood, the method was also applied to corresponding samples purchased from a supermarket. The methylated lead fraction in these samples, correlated to total lead, varied over a broad range (from 0.01% to 7.6%). On the other hand, the MeHg+ fraction was much higher, normally in the range of 80–100%. Considering that we may expect tighter legislative limitations on MeHg+ levels in seafood in the future, we found the highest methylmercury contents (up to 10.6 μg g−1) in two shark samples, an animal which is at the end of the marine food chain, whereas MeHg+ contents of less than 0.2 μg g−1 were found in most other seafood samples; these results correlate with the idea that MeHg+ is usually of biological origin in the marine environment. The concentration of butyltins and the fraction of the total tin content that is from butyltins strongly depend on possible contamination, due to the exclusively anthropogenic character of these compounds. A broad variation in the butylated tin fraction (in the range of <0.3–49%) was therefore observed in different seafood samples. Corresponding isotope-labeled spike compounds (except for trimethyllead) are commercially available for all of these compounds, and since these can be used in the multi-species species-specific GC-ICP-IDMS method developed here, this technique shows great potential for routine analysis in the future.  相似文献   

20.
Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion blank for Pb was reduced to 0.21 ng g−1 after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 ± 0.8 ng g−1 (mean ± expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 ± 3 ng g−1 and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a, NIES CRM 10-a, and NIES CRM 10-b, were 7.32 ± 0.24 ng g−1 (n = 5), 1010 ± 10 ng g−1 (n = 5), and 1250 ± 20 ng g−1 (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the National Metrology Institute of Japan (NMIJ) was observed to be 4.36 ± 0.28 ng g−1 (n = 10 bottles). Figure Digestion blank of Pb was carefully reduced to approximately 0.2 ng g-1 which permitted the highly precise determination of Pb at low ng g-1 level in foodstuff samples by ID-SFMS  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号