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LC-MS quantification of drug metabolites is sometimes impeded by the availability of internal standards that often requires customized synthesis and/or extensive purification. Although isotopically labeled internal standards are considered ideal for LC-MS/MS based quantification, de novo synthesis using costly isotope-enriched starting materials makes it impractical for early stage of drug discovery. Therefore, quick access to these isotope-enriched compounds without chemical derivatization and purification will greatly facilitate LC-MS/MS based quantification. Herein, we report a novel 18O-labeling technique using metabolizing enzyme carboxylesterase (CES) and its potential application in metabolites quantification study. Substrates of CES typically undergo a two-step oxygen exchange with H218O in the presence of the enzyme, generating singly- and doubly-18O-labeled carboxylic acids; however, unexpected hydrolytic behavior was observed for three of the test compounds – indomethacin, piperacillin and clopidogrel. These unusual observations led to the discovery of several novel hydrolytic mechanisms. Finally, when used as internal standard for LC-MS/MS based quantification, these in situ labeled compounds generated accurate quantitation comparable to the conventional standard curve method. The preliminary results suggest that this method has potential to eliminate laborious chemical synthesis of isotope-labeled internal standards for carboxylic acid-containing compounds, and can be developed to facilitate quantitative analysis in early-stage drug discovery.  相似文献   
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The main objective of this study was to examine the psychosocial stress model developed by Taylor and Aspinwall with emotional exhaustion as the outcome variable. Respondents, 409 men and 346 women, who had a paid job for at least 20 hours per week, completed questionnaires concerning demographic variables, personality, temperament, work pressure, workload, perceived social support, appraisal, coping, and emotional exhaustion. Structural equation analyses provided only partial support for the validity of the model. First, on theoretical and statistical grounds, one more path linking external resources to social support was added. Second, contrary to expectations, coping styles did not predict emotional exhaustion. To conclude, when coping is measured retrospectively, it does not add to our understanding of emotional exhaustion. It is suggested that future studies should be longitudinal and include objective measures of stressors and psychosocial health outcomes in addition to self‐reports. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   
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BACKGROUND: Gastric bypass is an established bariatric procedure that has undergone multiple modifications to improve its effectiveness. The side-to-side stapled technique is well recognized, but closure of the gastrotomy/enterotomy by the stapler can potentially narrow the Roux limb. Because of this, many surgeons will hand suture the closure of the gastrotomy/enterotomy. To obviate this difficulty, we inserted the linear stapler from the stomach's greater curvature, using a double-stapled anastomosis that minimized the need for hand suturing. METHODS: We performed a retrospective analysis of 307 patients undergoing this technique for laparoscopic gastric bypass. The weight loss and 30-day morbidity and mortality were tabulated and compared with those in other published series. RESULTS: Of the 307 patients, none died postoperatively. The overall 30-day morbidity rate was 15%. Two leaks from the gastrojejunostomy and 2 from the jejunojejunostomy (1.2%) developed. The mean percentage of excess weight loss was 34% at 3 months, 52% at 6 months, 73% at 1 year, 71% at 2 years, and 69% at 3 years. CONCLUSION: The greater curve approach avoids Roux limb obstruction, minimizes the need for hand suturing, and uses standard trocar incisions. Our short-term follow-up results are similar to those of series of other techniques.  相似文献   
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辛伐他汀对人低密度脂蛋白氧化修饰影响的实验研究   总被引:2,自引:2,他引:0  
目的研究辛伐他汀在体外对低密度脂蛋白氧化修饰的影响.方法以低密度脂蛋白氧化修饰为模型,以硫代巴比妥酸反应物质(TBARS)生成量及相对电泳迁移率(REM)为指标,研究了辛伐他汀对铜离子(Cu2 )诱导低密度脂蛋白氧化修饰的抑制作用.结果随辛伐他汀浓度从1~10μmol/L的增加,TBARS值分别减少67.3%,73.9%,81.9%,REM值减少48.3%,55.2%,58.6%,呈浓度及时间依赖关系.其中10μmol/L辛伐他汀可几乎完全抑制低密度脂蛋白氧化.结论辛伐他汀在体外能明显抑制Cu2 诱导的低密度脂蛋白氧化修饰.  相似文献   
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通过溴化聚苯醚和格利雅试剂反应,将不饱和基团烯丙基引入聚苯醚中实现其热固性改性,由^1H-NMR和FTIR进行结构表征。确定了烯丙化聚苯醚的固化工艺,并对其固化产物性能进行测试。结果表明:按合成新工艺制备的热固性聚苯醚,其固化产物具有优异的介电性能(低介电常数、低介电损耗因子),良好的耐溶剂性能和低吸湿性。  相似文献   
8.
To determine the structural perturbations induced by the CαH→Nα exchange in aza-peptides, we have examined by H NMR and IR spectroscopy various derivatives of the aza-analogues of alanine, aspartic acid and asparagine in different organic solvents with increasing polarity. Their general formulas are: R'-AzXaa-NR2R3, R'-Pro-AzXaa-NR2R3 and R-AzXaa-Pro-NR2R3 (where AzXaa denotes the aza-analogue of the amino acid residue Xaa = Ala, Asp, Asn; R = Boc, Z; R2, R3= H, Me, iPr). The aza-analogue of an amino acid residue appears to be a strong p-turn-inducing motif, and the AzAsn carboxamide side-chain is capable of interacting, as a proton donor, with the preceding peptide carbonyl group.  相似文献   
9.
建立了较完整的估计重油和沥青中饱和碳浓度数方法,其中包括环烷桥头碳、环烷甲基取代碳、环烷烷基(≥C2)取代碳等。基于理论分析,建立了估计环间的桥链和各种平均结构参数的方法,包括平均芳环环核数和环烷环环核数、芳环和环烷环烷工取代度、单元片上芳环和环烷环数。从实验数据出发,提出了烷基链长分布的公式。  相似文献   
10.
BACKGROUND: Allergoids are widely used in specific immunotherapy (SIT) for the treatment of IgE-mediated allergic diseases, but all techniques for standardization of conventional allergic extracts may not be appropriate for standardization of a glutaraldehyde (GA)-modified extract because of the unique characteristics of these extracts. OBJECTIVE: To assess an accurate methodology for standardization of chemically modified extracts. METHODS: GA-modified extracts from Parietaria judaica pollen were purified by diafiltration. Biochemical properties were investigated by determination of amino groups, chromatography, and SDS-PAGE. The IgE-binding activity was determined by skin prick test, enzyme allergosorbent test inhibition, basophil activation, and histamine release tests. Peripheral blood mononuclear cells (PBMCs) from P. judaica pollen-allergic subjects were stimulated with either native or allergoid extracts, and proliferation was measured. RESULTS: Biochemical data indicated a high degree of allergen polymerization resulting in extract components higher than 100 kDa. IgE-binding activity, both in vivo and in vitro, was reduced by more than 99.8%. Both allergen and allergoid induced PBMC proliferation and synthesis of blocking IgG antibodies at similar rates. Moreover, no evidence of introduction of new determinants by chemical modification was found. CONCLUSIONS: The preparation of GA-modified extracts by diafiltration is faster and more reliable than previous chromatographic methods. These modified extracts have drastically reduced their allergenicity while maintaining their immunogenicity, and therefore they can be used in safer and shortened schedules of SIT.  相似文献   
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