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Cinabro D Henderson S Kinoshita K Liu T Saulnier M Wilson R Yamamoto H Sadoff AJ Ammar R Ball S Baringer P Coppage D Copty N Davis R Hancock N Kelly M Kwak N Lam H Kubota Y Lattery M Nelson JK Patton S Perticone D Poling R Savinov V Schrenk S Wang R Alam MS Kim IJ Nemati B O'Neill JJ Romero V Severini H Sun CR Zoeller MM Crawford G Fulton R Fujino D Gan KK Kagan H Kass R Lee J Malchow R Morrow F Skovpen Y Sung M White C Whitmore J Wilson P Butler F Fu X Kalbfleisch G Lambrecht M Ross WR 《Physical review letters》1993,70(24):3700-3704
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Syntheses of 5-isopropyl-1,3-cyclohexadiene and syn-5-isopropyl-2,3-dioxabicyclo[2.2.2]octane, by routes that would allow completely diastereoselective introduction of deuterium labels, are described. The reaction of the isopropyl cyclohexadiene with singlet oxygen is shown to give an endoperoxide that is derived by preferential attack on the more sterically hindered face of the diene. A possible mechanistic explanation of this result is that the attack from the less hindered face leads to "ene" reaction rather than endoperoxide formation. However, this mechanism would require that the "ene" reaction and cycloaddition proceed via a common intermediate-presumably a perepoxide. 相似文献
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A high-performance liquid chromatographic method is described for the determination of terbutaline in human plasma in the range 1-35 ng/ml. Detection was achieved using a carbon fibre micro-electrochemical detector and a column-switching system. The microelectrode cell has advantages over conventional glassy carbon electrode-based detection systems in that it is easy to prepare, flexible in its operation and suffers less trouble from problems such as air bubbles and leaks. Furthermore, it has a better detection limit for terbutaline (0.8 ng/ml) to that obtained using a conventional glassy carbon electrode flow detector (2 ng/ml). Sample clean-up was by on-line solid-phase extraction with column switching, providing a method which was sensitive and reproducible, where the mean overall coefficient of variation was 5.60% and drug recovery in excess of 86% at the concentration levels studied. 相似文献
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The present work describes a metallic hydride atomizer for atomic absorption spectrometry, by evaluating the performance of the Inconel 600® tube. For this purpose, stibine was used as the model volatile compound and antimony determination in river and lake sediments and in pharmaceutical samples was carried out to assess the metal furnace performance. Some parameters are evaluated such as those referring to the generation and transport of the hydride (such as KBH4 and acid concentrations, carrier gas flow rate, injected volume, etc.), as well as those referring to the metal furnace (such as tube hole area, flame composition, long-term stability, etc.). The method presents linear Sb concentration from 2 to 80 μg L−1 range (r > 0.998; n = 3) and the analytical frequency of ca. 140 h−1. The limit of detection (LOD) is 0.23 μg L−1 and the precision, expressed as R.S.D., is less than 5% (40 μg L−1; n = 10). The accuracy is evaluated through the reference materials, and the results are similar at 95% confidence level according to the t-test. 相似文献
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Gaucher disease-associated glucocerebrosidases show mutation-dependent chemical chaperoning profiles
Sawkar AR Adamski-Werner SL Cheng WC Wong CH Beutler E Zimmer KP Kelly JW 《Chemistry & biology》2005,12(11):1235-1244
Gaucher disease is a lysosomal storage disorder caused by deficient glucocerebrosidase activity. We have previously shown that the cellular activity of the most common Gaucher disease-associated glucocerebrosidase variant, N370S, is increased when patient-derived cells are cultured with the chemical chaperone N-nonyl-deoxynojirimycin. Chemical chaperones stabilize proteins against misfolding, enabling their trafficking from the endoplasmic reticulum. Herein, the generality of this therapeutic strategy is evaluated with other glucocerebrosidase variants and with additional candidate chemical chaperones. Improved chemical chaperones are identified for N370S glucocerebrosidase. Moreover, we demonstrate that G202R, a glucocerebrosidase variant that is known to be retained in the endoplasmic reticulum, is also amenable to chemical chaperoning. The L444P variant is not chaperoned by any of the active site-directed molecules tested, likely because this mutation destabilizes a domain distinct from the catalytic domain. 相似文献