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1.
Acta Chir Orthop Traumatol Cech ; 91(1): 17-23, 2024.
Artigo em Tcheco | MEDLINE | ID: mdl-38447561

RESUMO

PURPOSE OF THE STUDY: Spine stabilization surgery is nowadays one of the most common spinal surgical procedures. Spinopelvic alignment is considered to be an important factor impacting the patients' preoperative diffi culties as well as the outcome of surgery. In our study, the outcomes of stabilization surgeries in patients with lumbar spine disorders were evaluated - especially in those with stenosis and spondylolisthesis, in whom the importance of sagittal parameters were assessed with respect to the patients' clinical outcomes and diffi culties. MATERIAL AND METHODS: The study included 50 patients with lumbar spine disorders who had undergone a spine stabilization surgery for a degenerative disease - lumbar spinal stenosis, spondylolisthesis between 2015 and 2017. Spino-pelvic radiological parameters and clinical parameters were evaluated using the nonparametric Kruskal-Wallis, Mann-Whitney, and Wilcoxon tests. RESULTS: In 38 of 50 patients, who at the end of the follow-up period did not have the PI-LL (pelvic incidence-lumbar lordosis) mismatch, i.e. PI-LL was ≤10°, a statistically signifi cant difference in pelvic tilt (p=0.049) and sagittal vertical axis (p<0.001) was reported, which was not the case in the remaining patients of the study population. Claudication and OSWESTRY (ODI) showed no statistically signifi cant difference. We have also compared the differences in the number of fused vertebrae and type of stabilization. A signifi cant change was seen in the claudication parameter at 12 and 24 months after surgery (p=0.007, p=0.005), with better outcomes achieved by 360° lumbar fusion compared to posterior lumbar fusion. The improvement of VAS and ODI scores in both the groups over time (from 6.1 to 3.6 or from 6.3 to 3.5 in VAS and from 62 to 32, or from 62 to 30 in ODI) was also statistically signifi cant (p<0.001 in both groups), while when comparing the groups against each other it was statistically insignifi cant. DISCUSSION: The authors confi rmed signifi cant improvement in the studied clinical parameters in all groups of patients (VAS, ODI, claudication), which is consistent with the results of recently published papers. The authors also established the correlation between different radiological parameters in the studied groups. The results do not confi rm the importance of the length or type of instrumentation for the clinical outcomes. This is consistent with the fi ndings of other published manuscripts. The authors failed to confi rm a signifi cant change in clinical parameters in dependence on the matching relationship between the pelvic incidence and lumbar lordosis. CONCLUSIONS: Proper spinopelvic balance in patients after spinal surgery is a very important indicator of postoperative development and condition, but our cohort showed no statistically signifi cant difference in the clinical outcomes of patients whose postoperative sagittal parameters were unsatisfactory. KEY WORDS: sagittal profi le, spine stabilization, pelvic tilt, pelvic incidence, sagittal vertical axis, SVA.


Assuntos
Lordose , Espondilolistese , Animais , Humanos , Espondilolistese/cirurgia , Coluna Vertebral , Marcha , Procedimentos Neurocirúrgicos
2.
J Proteomics ; 140: 55-61, 2016 05 17.
Artigo em Inglês | MEDLINE | ID: mdl-27063990

RESUMO

UNLABELLED: Although several new biomarkers have been recently proposed for psoriasis (Ps) and psoriasis arthritis (PsA), nothing is known about their diagnostic sensitivity and specificity, and their routine use. We therefore searched in-depth for new biomarker candidates using a biobank with EDTA-plasma from 158 individuals, patients and healthy controls. Samples from 6 selected pairs (patients against healthy controls) were searched proteomically using a workflow of extensive and precise design that is highly comprehensive. Subsequent verification was performed using ELISA and the entire biobank. By proteomic methods, 208 altered proteins were identified. Of these, 15 biomarker candidates were selected for verification. Of these 15, 4 individual parameters and 11 combinations significantly discriminated between patient and control groups. These individual parameters were Zn-α2-glycoprotein, complement C3, polymeric immunoglobulin receptor, and plasma kallikrein. Significant discrimination was obtained by combinations of 2 or 3 parameters. One combination seemed suitable for diagnosing PsA. Moreover, several candidates desmoplakin, complement C3, polymeric immunoglobulin receptor, and cytokeratin 17, correlated with PASI in all patients. This first comprehensive proteomic study on non-depleted plasma identified several biomarker candidates that have not been described before as well as some known from previous studies. BIOLOGICAL SIGNIFICANCE: Our non-gel proteomic analysis is based on the highly comprehensive and significantly optimized chromatographic protein pre-fractionation. The method allows a biomarker search in non-depleted plasma. The subsequent verification by ELISA identifies several biomarker-candidates for the unbiased diagnosis of psoriasis and psoriasis arthritis. Four of the identified candidate markers might be used individually. Combinations of several parameters improve the diagnostic sensitivity and specificity. The still not validated candidates form a reserve for further evaluation. Moreover, mass spectrometric data uncover several biomarker-candidates which show diverse protein species of the same protein with opposing changes in the same sample.


Assuntos
Artrite Psoriásica/diagnóstico , Proteômica/métodos , Psoríase/diagnóstico , Adulto , Artrite Psoriásica/sangue , Biomarcadores , Estudos de Casos e Controles , Complemento C3/análise , Desmoplaquinas/sangue , Feminino , Glicoproteínas/sangue , Humanos , Queratina-17/sangue , Masculino , Espectrometria de Massas , Pessoa de Meia-Idade , Calicreína Plasmática/análise , Psoríase/sangue , Receptores de Imunoglobulina Polimérica/sangue
3.
Artigo em Inglês | MEDLINE | ID: mdl-23906762

RESUMO

Multidimensional chromatographic separation for proteomic biomarker search generates sets of several hundred homologous fractions, which have to be compared. Due to the high number of sequential steps, deviations between samples may be produced randomly by slight processing differences. These deviations may falsify proteomic results. In order to overcome this problem, we tested the applicability of quality control by colored phycobilins as internal standards. The elution of the used protein standards themselves shows a high reproducibility since their main peak location is practically constant under proper performance of size exclusion and anion exchange chromatography. This applies to runs of one phycobilin alone, combined with another phycobilin, or combined with plasma proteins. Thus, these protein standards do not disturb sample processing. Characteristic peak shifts of phycobilins allow easy observation of deviations caused by typical failures in the elution protocol (aberrant step number, buffer permutation). Mass spectrometric analysis is not influenced by their presence since protein coverage, peptide numbers, and protein numbers are not altered. Thus, colored protein standards may be used for quality control and evaluation of robustness of various chromatographic applications.


Assuntos
Cromatografia em Gel/normas , Cromatografia por Troca Iônica/normas , Proteômica/normas , Proteínas Sanguíneas/análise , Peptídeos/isolamento & purificação , Ficobilinas/análise , Proteínas/isolamento & purificação , Proteômica/métodos , Controle de Qualidade , Padrões de Referência
4.
Acta Chir Orthop Traumatol Cech ; 76(6): 501-4, 2009 Dec.
Artigo em Tcheco | MEDLINE | ID: mdl-20067698

RESUMO

PURPOSE OF THE STUDY: We present a group of patients with spinal metastatic disease surgically treated at our department, with an evaluation of their neurological outcomes in relation to the initial disease and the surgical technique used. MATERIAL: Between 1989 and 2007 we operated on 748 patients with spinal tumour. Of these, 380 had metastatic disease. The Frankel classification system was used to assess neurological status. METHODS: Based on the Tomita prognostic score, the metastatic disease was evaluated and appropriate surgical procedure was selected (biopsy, posterolateral decompression, posterolateral decompression with stabilisation, somatectomy, or vertebrectomy/spondylectomy). The neurological findings before and after surgery and at follow-up were assessed. RESULTS: Of the 368 patients evaluated, four were pre-operatively classified as Frankel grade A, 29 as grade B, 99 as grade C, 82 as grade D and 159 patients as grade E. Post-operative outcomes were: Frankel grade A, 6 patients B, 27 C, 78 D, 79 and E, 178 patients. Surgery resulted in neurological deterioration by 3 degrees of the Frankel scale in two patients (0.5%), 2 degrees in three patients (0.8%), and by 1 degree in 17 patients (4.6%). Improvement was recorded: by 1 degree in 57 patients (15.5%), 2 degrees in 10 (2,7%) and 3 degrees in two patients (0.5%). Of 23 patients who underwent biopsy, neurological status improved in one (4.3%) and deteriorated also in one patient (4.3%). Of the 85 patients treated by posterolateral decompression, improvement was recorded in 25 (29.4%) and deterioration in two (2.4%). Of the 73 patients undergoing posterolateral decompression with stabilisation, neurological findings improved in 15 (17.9%) and deteriorated in five (6.0%). In the group of 103 patients treated by vertebrectomy, neurological findings improved in 13 (12.6%) and deteriorated in eight (7.8%). At an average follow-up of 15 months, 208 (55.7%) patients presented themselves of these, improvement in neurological status was recorded in 16 (7.8%) and deterioration in eight (3.9%), as compared with the pre-operative values. DISCUSSION: Any comparison with the literature data is difficult, because both the criteria of indication for surgery and the method of treatment differ considerably. Improvement in neurological status was achieved in 69 patients (18.8%). CONCLUSIONS: Metastatic tumours of the spine present a serious diagnosis, with pain often being the first sign of a malignant disease. The degree of neurological deficit, primary tumour site and the extent of metastatic spinal disease (objectively evaluated on the basis of the Tomita score) should determine whether the patient will be operated on or not and, if so, whether a radical or mere palliative procedure will be used. An important factor is multidisciplinary cooperation of attending physicians both preoperatively and during the post-operative care of cancer patients.


Assuntos
Doenças do Sistema Nervoso/etiologia , Neoplasias da Coluna Vertebral/secundário , Neoplasias da Coluna Vertebral/cirurgia , Adolescente , Adulto , Idoso , Idoso de 80 Anos ou mais , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Doenças do Sistema Nervoso/diagnóstico , Neoplasias da Coluna Vertebral/fisiopatologia , Adulto Jovem
5.
Acta Chir Orthop Traumatol Cech ; 75(3): 180-4, 2008 Jun.
Artigo em Tcheco | MEDLINE | ID: mdl-18601815

RESUMO

PURPOSE OF THE STUDY: In a retrospective study, to analyze long-term radiographic results of two surgical procedures used to treat congenital scoliosis. MATERIAL AND METHODS: A total of 685 patients with congenital scoliosis were treated at the Department of Orthopaedic Surgery, Bohunice Teaching Hospital in Brno, between 1976 and 2007. Of these, 102 patients, with an average age of 6.6 years at the time of surgery, were treated by simple bony fusion, and 22 children, with an average age of 10.2 years, underwent instrumented hemivertebra excision via simultaneous anterior and posterior exposures involving fixation with cannulated compression screws and a wire loop. The follow-up periods for the former and latter groups were 14.2 and 12.1 years, respectively. RESULTS: In the patients treated by simple bony fusion, the mean correction rate was 22.1 %, with Cobb angle values averaging from 44.2 degrees pre-operatively to 38 degrees post-operatively; the correction loss was 3.9 degrees at the last follow up. In the patients with hemivertebra excision, the mean correction rate was 61 %, with pre- and post-operative values of 51.3 degrees and 20.3 degrees , respectively, and a correction loss of 1.1 degrees at the last follow-up. DISCUSSION: The early detection of a deformity and simple bony fusion in low-magnitude curves can prevent progression of scoliosis and allows for maintenance of a compensated spine. Hemivertebra excision with compression instrumentation results in a better surgical correction of the deformity. The average 61 % correction rate achieved in our patients is in agreement with the results reported by authors using the same surgical technique, as well as with the results of posterior hemivertebra resection. The best correction, 78 %, has been achieved with surgery at a very young age. Complications associated with the two techniques are rare. CONCLUSIONS: Congenital scoliosis due to failure off either formation or segmentation is indicated for surgical treatment at young age. Its early detection and subsequent surgical treatment at young age. Its early detection and subsequent surgical correction of the curve result in a long-term maintenance of a compensated spine. Instrumented hemivertebra excision provides the highest rate of correction, particularly if carried out before 3 years of age.


Assuntos
Vértebras Lombares/cirurgia , Escoliose/congênito , Escoliose/cirurgia , Fusão Vertebral , Vértebras Torácicas/cirurgia , Adolescente , Criança , Pré-Escolar , Feminino , Humanos , Lactente , Masculino , Radiografia , Escoliose/diagnóstico por imagem
6.
Cent Eur J Public Health ; 13(3): 153-8, 2005 09.
Artigo em Inglês | MEDLINE | ID: mdl-16218333

RESUMO

Mining for coal and its utilization have various impacts on the surrounding environment. Huge volumes of waste materials which are by-products of both the underground and open cast coal mining, pose one of the major environmental hazards in addition to air pollution caused by coal burning in power plants in the Czech Republic. Some of these risks could be reduced when having accurate and comprehensive data on coal quality. Statistical data processing of almost 35,000 coal samples from Late Paleozoic and Tertiary coal basins of the Czech Republic provided a unique information on the quality of lignite, sub-bituminous and bituminous coals and anthracites including the content of toxic trace elements (As, Be, Hg, Pb and Se). In this context related environment and health risks and protection implications are discussed.


Assuntos
Poluentes Atmosféricos/efeitos adversos , Carvão Mineral/efeitos adversos , Exposição Ambiental/efeitos adversos , Oligoelementos/efeitos adversos , Poluentes Atmosféricos/análise , Arsênio/efeitos adversos , Arsênio/análise , Berílio/efeitos adversos , Berílio/análise , Carvão Mineral/análise , República Tcheca , Exposição Ambiental/estatística & dados numéricos , Humanos , Chumbo/efeitos adversos , Chumbo/análise , Mercúrio/efeitos adversos , Mercúrio/análise , Centrais Elétricas , Selênio/efeitos adversos , Selênio/análise , Oligoelementos/análise
7.
J Anim Sci ; 81(5): 1348-53, 2003 May.
Artigo em Inglês | MEDLINE | ID: mdl-12772863

RESUMO

Since 1989, an undergraduate course addressing issues concerning biotechnology in agriculture has been taught annually. To determine the extent to which students were engaged in classroom instruction and assimilated knowledge from the course, students were asked to complete an "Attitudes About Biotechnology" questionnaire. Students were queried about their knowledge of biotechnology, perceptions of risks associated with biotechnology, and ethics and attitudes toward the use of biotechnology in agriculture. Responses to the survey questions were evaluated both pre-and postcourse. Data were collected from 13 classes over a 10-yr period. Inspection of the precourse grade point average and the course grades for these students revealed no trends up or down over the period of this study. Similarly, inspection of the data revealed no effect from problem-based learning, student-facilitated group work, or technology on student attainment of knowledge, perception of risk, or ethical views. For each of the five knowledge questions, the average score increased as a result of taking the course. On two of the knowledge questions, the average score increase for females from pre- to postcourse was greater than for males. Based on our measurements using the postcourse questionnaire, the correlation between perceived and actual knowledge was not significantly different from zero. In two of the four risk questions, there was no change in average score as a result of the course; however, student perception of risk associated with genetic engineering of plants increased. Although average scores for student perception of risk due to the perceived impact of genetically engineered products on people or the environment decreased from pre- to postcourse assessment, the average score was higher (P < 0.01) for females than for males. Males were more accepting of genetic manipulation of cells in a laboratory than were females both pre- and postcourse. Although student knowledge of biotechnology was increased and the perceived risk due to biotechnology was altered, there was no evidence that students altered their ethical position on biotechnology as a result of this course.


Assuntos
Biotecnologia , Percepção , Estudantes/psicologia , Adulto , Biotecnologia/educação , Biotecnologia/ética , Avaliação Educacional , Feminino , Conhecimentos, Atitudes e Prática em Saúde , Humanos , Masculino , Plantas Geneticamente Modificadas , Fatores de Risco , Distribuição por Sexo , Inquéritos e Questionários
8.
Anal Chem ; 73(21): 5116-25, 2001 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-11721908

RESUMO

In this paper, we report on investigations related to the performance characteristics of two different types of etched chemically (n-octadecyl- and cholesterol-) modified capillaries in the open tubular format of capillary electrochromatography (CEC) for the analysis of synthetic peptides. The results confirm that the nature of the surface chemistry used to modify the capillary wall and type of chemically bonded group employed can affect the selectivity as well as the resolution of peptide samples. The results are consistent with the participation of selective peptide interactions with the bonded phase, although other factors, such as the morphology of the capillary wall surfaces, appear to be also involved. Moreover, several surprising observations related to peptide-specific multi-zoning effects have been observed. Additional experimental variables that can also be utilized to affect the retention of peptides in this approach to OTCEC include the type and percentage of organic solvent modifier employed in the eluent and the pH of the buffer system. To evaluate the reproducibility of different batches of the n-octadecyl- and cholesterol-modified capillaries and the stability of the chemically modified surface, the OTCEC selectivity and peak shape behavior of two small basic molecules (serotonin and tryptamine) and two proteins (turkey and chicken lysozyme) were also investigated. Finally, the use of the "bubble" cell technology for creating the detector window has been shown to provide significantly higher detection sensitivity with peptides, as compared with the conventional capillary format.


Assuntos
Cromatografia Capilar Eletrocinética Micelar/métodos , Eletroforese Capilar/métodos , Peptídeos/análise , Peptídeos/síntese química , Sequência de Aminoácidos , Animais , Galinhas , Colesterol , Proteínas de Choque Térmico HSP90/análise , Dados de Sequência Molecular , Muramidase/análise , Reprodutibilidade dos Testes , Serotonina/análise , Triptaminas/análise , Perus
9.
Electrophoresis ; 22(12): 2620-8, 2001 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-11519968

RESUMO

In this article, the effects of the stationary phase, buffer pH, organic modifier type, organic modifier composition, applied voltage, and temperature on the migration of several synthetic peptides in etched chemically modified open-tubular capillaries are discussed. With these solutes, migration is due to two effects: electrophoretic mobility and solute/bonded phase interactions. In addition, relative migration rates are evaluated for the peptide samples as a function of these experimental variables in order to determine which parameters might be useful for optimizing separations in open-tubular capillary electrochromatography (OTCEC). Some examples of synthetic peptide separations are presented where the sample contains a major component and several minor species, demonstrating how the resolution of these mixtures can be affected by the appropriate choice of experimental variables.


Assuntos
Eletroforese Capilar/instrumentação , Alcenos , Amônia , Ésteres do Colesterol , Furanos , Concentração de Íons de Hidrogênio , Peptídeos/análise , Peptídeos/síntese química , Peptídeos/isolamento & purificação , Proteínas/análise , Proteínas/química , Proteínas/isolamento & purificação , Receptores de Trombina , Silanos , Dióxido de Silício , Solventes , Propriedades de Superfície , Temperatura
10.
J Chromatogr A ; 924(1-2): 211-21, 2001 Jul 27.
Artigo em Inglês | MEDLINE | ID: mdl-11521867

RESUMO

In this investigation, various capillary electrochromatographic (CEC) experiments have been employed to characterize the properties of etched, chemically-modified surfaces of open tubular capillary columns with peptides as solute probes and under conditions of variable voltage, temperature and solvent composition. The separation performance of etched capillaries with either n-octadecyl or liquid crystal moieties derived from a cholesterol phase bonded to the surface were compared. With the liquid crystal bonded species, interesting and significantly different variations in retention behavior of peptides are obtained compared to those observed with the corresponding n-octadecyl modified surfaces by changes in temperature, solvent composition and field strength. These peptide separations illustrate the usefulness of this CEC approach for practical applications, where both the retention characteristics of the charged analytes as well as the selectivity differences due to the surface properties of the etched chemically-modified surfaces of open tubular capillary columns can be rationally modulated. As in HPLC, appropriate choice of CEC experimental variables, including the chemical properties of the immobilized ligand(s), represents a powerful tool for optimizing resolution.


Assuntos
Cromatografia Capilar Eletrocinética Micelar/instrumentação , Peptídeos/química , Peptídeos/isolamento & purificação , Solventes , Temperatura
11.
Drug Metabol Drug Interact ; 18(3-4): 159-90, 2001.
Artigo em Inglês | MEDLINE | ID: mdl-11791883

RESUMO

Powerful medicinal properties have been recorded for Zingiber officinale, commonly known as ginger. All of these medicinal activities have been compiled with 99 references to the present status of the plant in the literature. Volatile components and the presence of trace metals are included. In addition, details of individual medicinal activities are given and the molecular structures of identified organic metabolites and their synthesis are described.


Assuntos
Fitoterapia/métodos , /química , Anticolesterolemiantes/uso terapêutico , Antioxidantes/uso terapêutico , Antirreumáticos/uso terapêutico , Pressão Sanguínea/efeitos dos fármacos , Cromatografia Gasosa/métodos , Humanos , Extratos Vegetais/uso terapêutico , Agregação Plaquetária/efeitos dos fármacos , Úlcera Gástrica/prevenção & controle , Oligoelementos/análise
12.
Metabolism ; 49(11): 1424-30, 2000 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-11092505

RESUMO

Lipoprotein and apolipoprotein changes were evaluated in 10-week-old Zucker diabetic fatty (ZDF) male rats following 12 weeks of insulin treatment, which normalized blood glucose and maintained weight gaining characteristic of nondiabetic Zucker fatty rats. Compared with untreated ZDF rats (saline-injected), insulin treatment resulted in increased very-low-density lipoprotein (VLDL; d < 1.006 g/mL) and decreased alpha lipoprotein on agarose gel electrophoresis. These findings were consistent with an observed increase in VLDL triglyceride and cholesterol, and decreased high-density lipoprotein (HDL) cholesterol with insulin treatment in isolated lipoproteins. B100 levels were unchanged by insulin treatment, but B48 levels were significantly increased in the VLDL fraction. Insulin treatment depressed apolipoprotein (apo) A-I levels in HDL, but had little effect on total apo E, apo A-IV, or apo C, although apo C was redistributed to the VLDL fraction. These results suggest that insulin treatment of ZDF rats normalizes hyperglycemia and prevents age-related changes in lipoprotein parameters associated with development of insulinopenic diabetes. Insulin therapy in ZDF rats thereby sustains the hyperlipidemic lipoprotein pattern associated with hyperinsulinemia and obesity.


Assuntos
Hipertrigliceridemia/complicações , Insulina/administração & dosagem , Obesidade/complicações , Animais , Glicemia/análise , Cromatografia em Gel , Eletroforese em Gel de Poliacrilamida , Hiperinsulinismo/sangue , Hiperinsulinismo/complicações , Hipertrigliceridemia/sangue , Lipoproteínas/sangue , Lipoproteínas/classificação , Lipoproteínas/isolamento & purificação , Masculino , Fenótipo , Ratos , Ratos Zucker
13.
J Chromatogr A ; 887(1-2): 31-41, 2000 Jul 28.
Artigo em Inglês | MEDLINE | ID: mdl-10961302

RESUMO

This review describes an open tubular approach to capillary electrochromatography (OTCEC) that first etches the inner surface of the fused-silica tube using ammonium hydrogen diflouride. This process can increase the inner surface area significantly. The new surface is then chemically modified to attach a bonded stationary phase using a silanization/hydrosilation reaction process. The surfaces are characterized spectroscopically by diffuse reflectance infrared Fourier transform and by electroosmotic flow measurements. Applications of OTCEC columns with C18, diol and chiral stationary phases are described.


Assuntos
Eletroforese Capilar/métodos , Grupo dos Citocromos c/análise , Eletroforese Capilar/instrumentação , Muramidase/análise , Dióxido de Silício/química
14.
J Chromatogr A ; 887(1-2): 479-87, 2000 Jul 28.
Artigo em Inglês | MEDLINE | ID: mdl-10961335

RESUMO

Packed column capillary electrochromatography (CEC), open-tubular CEC and microcolum liquid chromatography (LC) using a cholesteryl silica bonded phase have been studied to compare the retention behavior for benzodiazepines. It has been found that packed column CEC gives better resolution, faster analysis time than microcolumn LC for benzodiazepines maintaining similar selectivity except for some solutes which are charged species under the separation conditions. However, open-tubular CEC gave different selectivities to a larger extent for charged benzodiazepines from that which should be produced by the chromatographic properties of the cholesteryl silica phase. Charged species migration times are mainly influenced by electrophoretic mobility rather than the chromatographic interactions.


Assuntos
Benzodiazepinas/isolamento & purificação , Eletroforese Capilar/métodos , Cromatografia Líquida/métodos , Fatores de Tempo
15.
J Chromatogr A ; 887(1-2): 497-503, 2000 Jul 28.
Artigo em Inglês | MEDLINE | ID: mdl-10961337

RESUMO

The presence of the carcinogenic N-nitrosodiethanolamine (NDELA; CAS No. 1116-54-7) in cosmetic samples was determined using an etched, C18 modified capillary in the open-tubular capillary electrochromatography technique. A very simple extraction procedure leads to a sample matrix free from interferences. The calibration curve was created using UV detection at 214 nm. The detector response was linear in the range of 5-120 ppm total amount injected. Minimum detection limits (1 ppm NDELA injected on capillary) are suitable for screening a large number of cosmetic samples. Diethanolamine and triethanolamine precursors of nitrosamines are not detected at the wavelength used. Cosmetic samples were analyzed unspiked and after addition of 60 ppm of NDELA. In spiked samples recoveries varied from 94% (hand and body lotion) to 55% (lipstick sample). NDELA was found in unspiked samples of old (5-15 years old) cosmetics at concentrations of 14.0 ppm and 35.0 ppm.


Assuntos
Cosméticos/química , Dietilnitrosamina/análogos & derivados , Dietilnitrosamina/análise , Eletroforese Capilar/métodos , Contaminação de Medicamentos , Concentração de Íons de Hidrogênio , Espectrofotometria Ultravioleta/métodos
16.
J Chromatogr A ; 883(1-2): 55-66, 2000 Jun 23.
Artigo em Inglês | MEDLINE | ID: mdl-10910200

RESUMO

The temperature effect on the separation of fullerenes in LC was examined using monomeric type C30, C18 and C8 alkyl bonded stationary phases. It appears that the C30 phase exhibits superior separation ability for fullerenes. It is observed that the maximum retention temperature of fullerenes on the C30 phase is around 20 degrees C. A strong correlation between the changes in NMR spectra and the retention behavior of the solutes was found. The interpretation of the retention behavior of fullerenes on the alkyl bonded stationary phases, including the behavior in subambient temperature, is discussed using the information obtained by CP-MAS solid-state NMR spectroscopy and LC.


Assuntos
Carbono/isolamento & purificação , Cromatografia Líquida de Alta Pressão/instrumentação
17.
J Dairy Sci ; 83(7): 1479-86, 2000 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-10908056

RESUMO

We studied the effects of ammonia treatment on microbial populations during the fermentation of corn silage. We also compared the effects of ammonia to a preservative containing buffered propionic acid and other antifungal compounds on the fermentation and aerobic stability of corn silage. In the first experiment, whole-plant corn was ensiled without treatment or treated with ammonia-N to supply an additional 0.3% N (fresh-forage basis). The addition of ammonia immediately increased silage pH and had no effect on numbers of lactic acid bacteria, but delayed their growth compared with untreated silage. Numbers of enterobacteria declined more slowly, but numbers of yeasts and molds declined more quickly in silage treated with ammonia. During the early stages of ensiling, lactic acid increased more rapidly in untreated than in treated silage. The reverse was true for acetic acid concentrations. When exposed to air, growth of yeasts and molds was delayed in ammonia-treated silage. In a second experiment, various levels (0.1 to 0.3%, fresh weight) of ammonium-N or a preservative with buffered propionic acid were added to whole-plant corn and allowed to ensile for 106 d. Silage treated with ammonia had a greater ratio of L- to D-lactic acid than did other silages. Untreated silage was aerobically stable for 32.3 h, whereas the low (42 h) and moderate (52.7 h) concentrations of both additives numerically improved aerobic stability. High concentrations of ammonia-N (0.3%) or a buffered propionic acid preservative (0.3%), markedly improved the aerobic stability of corn silage (82 and 69 h for ammonia and propionic acid-treated silage, respectively).


Assuntos
Amônia/farmacologia , Fermentação , Conservantes de Alimentos/farmacologia , Propionatos/farmacologia , Silagem/microbiologia , Zea mays , Estabilidade de Medicamentos , Enterobacteriaceae , Concentração de Íons de Hidrogênio , Ácido Láctico/análise , Lactococcus , Oxigênio , Leveduras
18.
J Chromatogr A ; 853(1-2): 151-8, 1999 Aug 20.
Artigo em Inglês | MEDLINE | ID: mdl-10486721

RESUMO

The inner walls of 50 microns fused-silica capillaries are etched by ammonium hydrogendifluoride and then modified by the silanization/hydrosilation method with a chiral selector. Three different types of selectors were evaluated: lactone, beta-cyclodextrin and naphthylethylamine. Each of the bonded chiral stationary phases provided at least partial separation for one type of racemic solute. These results confirm that bonded organic moieties on the etched inner wall of a capillary can provided sufficient solute-bonded phase interactions to influence the retention of molecules driven through a capillary by electroosmosis or a combination of electroosmosis and electrophoretic mobility.


Assuntos
Cromatografia Capilar Eletrocinética Micelar/métodos , beta-Ciclodextrinas , Ciclodextrinas/química , Estudos de Viabilidade , Lactonas/química , Peptídeos/análise , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Estereoisomerismo
19.
Electrophoresis ; 20(12): 2343-8, 1999 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-10499324

RESUMO

A 50 microm capillary that has been etched with ammonium hydrogen difluoride is evaluated as a separation medium for capillary electrochromatography. For a tryptic digest of transferrin, the etched capillary gave better resolution (more peaks in the overall peptide map) and longer retention than separations done under identical experimental conditions on an unetched fused-silica capillary. Resolution on the etched capillary was improved by lowering the voltage from 300 to 267 V/cm. A four-component protein sample also resulted in longer retention on an echted capillary than on an unetched fused-silica capillary that were both coated with Polybrene. After correction for differences in electroosmotic flow between the two capillaries, the calculated electrophoretic mobilities for all four proteins were lower on the etched capillary than on the unetched fused-silica capillary. The results of both the tryptic digest and protein experiments strongly indicate the presence of chromatographic effects on the etched capillary that contribute to the increased retention and improved resolution with respect to the unetched fused-silica capillary.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Eletroforese Capilar/métodos , Peptídeos/isolamento & purificação , Proteínas/isolamento & purificação , Grupo dos Citocromos c/isolamento & purificação , Condutividade Elétrica , Brometo de Hexadimetrina , Muramidase/isolamento & purificação , Mioglobina/isolamento & purificação , Ribonuclease Pancreático/isolamento & purificação
20.
J Chromatogr A ; 845(1-2): 237-46, 1999 Jun 11.
Artigo em Inglês | MEDLINE | ID: mdl-10399338

RESUMO

Fused silica capillaries with an I.D. of 20 microns are etched and then chemically modified by the silanization/hydrosilation method to attach an octadecyl moiety for use in electrokinetic chromatography. The etched capillaries after chemical modification are shown to have an anodic electroosmotic flow below pH 4.5. In comparison to bare 20 microns capillaries and unetched but chemically modified 20 microns capillaries, the etched C18 fused silica tubes show better separation of mixtures of lysozymes and cytochrome c's under identical conditions of buffer, pH and applied voltage. It was also demonstrated that this open tubular approach to capillary electrochromatography was amenable to a number of different types of basic compounds ranging in size from typical small amines to biomolecules. As expected, pH is an important variable that must be controlled in order to obtain an optimized separation. Reproducibility studies verify the stability of the silicon-carbon linkage produced in this modification method so that column lifetimes of at least 300 injections can be expected.


Assuntos
Cromatografia/instrumentação , Cromatografia/métodos , Proteínas/isolamento & purificação , Ação Capilar , Grupo dos Citocromos c/isolamento & purificação , Eletroquímica , Concentração de Íons de Hidrogênio , Muramidase/isolamento & purificação , Osmose , Reprodutibilidade dos Testes , Dióxido de Silício
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