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71.
Madder A Li L De Muynck H Farcy N Van Haver D Fant F Vanhoenacker G Sandra P Davis AP De Clercq PJ 《Journal of combinatorial chemistry》2002,4(6):552-562
A series of peptidosteroid derivatives containing two independent peptide chains in which Ser and His are incorporated were synthesized by solid-phase peptide synthesis. The activity of the different compounds in the hydrolysis of the activated substrate NF31 was assessed in a stepwise fashion. First, the different resin-bound derivatives 6a-l and 6x-z were individually assayed for serine esterification in the absence of water. The use of a colored substrate allowed for a visual identification of the most active compounds. Through the inclusion of control substances, the involvement of histidine in the mechanism for serine acylation was shown. Second, the hydrolysis and methanolysis of the different acylated derivatives 8a-l and 8x were evaluated using UV spectroscopy, again indicating the involvement of histidine. The feasibility of applying the above procedures in a combinatorial context was proven via the screening of artificial libraries, created by mixing the different resin-bound peptidosteroid compounds. In this respect, the use of a photocleavable linker allowed for the unambiguous structural characterization of the selected members via application of single-bead electrospray tandem mass spectrometry. 相似文献
72.
Merel van Nuland Hilde Rosing Jan H.M. Schellens Jos H. Beijnen 《Biomedical chromatography : BMC》2020,34(1):e4623
Therapeutic drug monitoring (TDM) has shown to benefit patients treated with drugs of many drug classes, among which is oncology. With an increasing demand for drug monitoring, new assays have to be developed and validated. Guidelines for bioanalytical validation issued by the European Medicines Agency and US Food and Drug Administration are applicable for clinical trials and toxicokinetic studies and demand fully validated bioanalytical methods to yield reliable results. However, for TDM assays a limited validation approach is suggested based on the intended use of these methods. This review presents an overview of publications that describe method validation of assays specifically designed for TDM. In addition to evaluating current practice, we provide recommendations that could serve as a guide for future validations of TDM assays. 相似文献
73.
Total Synthesis of Δ12‐Prostaglandin J3: Evolution of Synthetic Strategies to a Streamlined Process 下载免费PDF全文
Prof. Dr. K. C. Nicolaou Dr. Kiran Kumar Pulukuri Ruocheng Yu Dr. Stephan Rigol Dr. Philipp Heretsch Dr. Charles I. Grove Christopher R. H. Hale Dr. Abdelatif ElMarrouni 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(25):8559-8570
The total synthesis of Δ12‐prostaglandin J3 (Δ12‐PGJ3, 1 ), a reported leukemia stem cell ablator, through a number of strategies and tactics is described. The signature cross‐conjugated dienone structural motif of 1 was forged by an aldol reaction/dehydration sequence from key building blocks enone 13 and aldehyde 14 , whose lone stereocenters were generated by an asymmetric Tsuji–Trost reaction and an asymmetric Mukaiyama aldol reaction, respectively. During this program, a substituent‐governed regioselectivity pattern for the Rh‐catalyzed C?H functionalization of cyclopentenes and related olefins was discovered. The evolution of the synthesis of 1 from the original strategy to the final streamlined process proceeded through improvements in the construction of both fragments 13 and 14 , exploration of the chemistry of the hitherto underutilized chiral lactone synthon 57 , and a diastereoselective alkylation of a cyclopentenone intermediate. The described chemistry sets the stage for large‐scale production of Δ12‐PGJ3 and designed analogues for further biological and pharmacological studies. 相似文献
74.
Sigve Sporst⊘l Kjell Urdal Hilde Drangsholt Nina Gj⊘s 《International journal of environmental analytical chemistry》2013,93(1-2):129-138
Abstract A method for automated determination of 73 organic pollutants in water is described. The compounds, which are key representatives for different types of pollutants are determined in two chromatographic runs. 11 halogenated aliphatic hydrocarbons are determined using capillary GC equipped with electron capture detector. The remaining pollutants, representing both basic/neutral and acidic compounds are determined by using GC/MS combined with an automated search computer program. The majority of the compounds have a limit of quantitation at 1 ig/1 or lower. The precision of the GC method is in the range of 1.8% to 4.3%, with an average of 3.2%. The precision for compounds determined by GC/MS is in the range of 1% to 38%, with an average of 14%. So far 30 water samples representing both polluted fjord areas as well as effluents from municipal treatment plants, refineries, petrochemical industries and metallurgic industries have been analysed. The method has been found to be an interesting alternative to traditional methods for monitoring water quality, and has demonstrated its potential both as a screening method for detecting “hot spots” as well as for routine monitoring of specific hazardous compounds. 相似文献
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76.
W. J. Agnew W. Böttger F. Feigl J. M. Kolthoff L. Michaelis S. Yamaguchi A. Martini L. Rosenthaler J. Kapulitzas F. Fröhnke R. Nakaseko Matsuy G. Denigès A. Benedetti-Pichler F. Schneider Hilde Thurnwald L. de Brouckère E. Belcke E. W. Schwartze R. M. Hann J. H. Yoe W. L. Hill J. L. Steenkamp K. Heller P. Krumholz R. Montequi W. H. Hammond R. Ripan G. Lode Fr. Hecht und W. Reich-Rohrwig 《Fresenius' Journal of Analytical Chemistry》1932,88(3-4):128-136
Ohne Zusammenfassung 相似文献
77.
W. J. Agnew W. Böttger F. Feigl J. M. Kolthoff L. Michaelis S. Yamaguchi A. Martini L. Rosenthaler J. Kapulitzas F. Fröhnke R. Nakaseko Matsuy G. Denigès A. Benedetti-Pichler F. Schneider Hilde Thurnwald L. de Brouckère E. Belcke E. W. Schwartze R. M. Hann J. H. Yoe W. L. Hill J. L. Steenkamp K. Heller P. Krumholz R. Montequi W. H. Hammond R. Ripan G. Lode Fr. Hecht W. Reich-Rohrwig 《Analytical and bioanalytical chemistry》1932,88(3-4):128-136
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