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71.
72.
Silvia Gaspa;Andrea Porcheddu;Antonio Valentoni;Sebastiano Garroni;Stefano Enzo;Lidia De Luca; 《European journal of organic chemistry》2017,2017(37):5519-5526
A mild, efficient, metal- and solvent-free oxidation of primary amines to aldehydes, ketones, and nitriles under ball-milling conditions is presented. This method has proved to be compatible with various functional groups and only requires easily accessible starting materials. Simple purification of the reaction mixtures by short-column chromatography afforded pure aldehydes, ketones, and nitriles as products. 相似文献
73.
Monique Zangarini Laura Ceriani Ezia Bello Giovanna Damia Roberta Cereda Maria Gabriella Camboni Massimo Zucchetti 《Journal of mass spectrometry : JMS》2014,49(1):19-26
We developed and validated a high‐performance liquid chromatography–tandem mass spectrometry analytical method to measure E‐3810, a novel dual inhibitor of fibroblast growth factor receptor 1 and vascular endothelial growth factor receptor 1–3 in tissues and determined the drug concentration in a biopsy of human breast cancer for the first time. The method is a modification of our previous one in plasma to study the clinical pharmacokinetics of the drug during the phase I/II trial. In view of the changes in matrix, we applied a partial validation protocol to determine recovery, sensitivity, range of linearity, precision, accuracy and stability of the method over three runs in a mouse tumor tissue and liver. The recovery of E‐3810 from liver or tumor homogenate was >69%, and the lower limit of quantification was 5 ng/ml. The method was linear in the concentration range 5.0–500.0 ng/ml, as demonstrated by a determination coefficient R2 ≥ 0.9955. The range of the calibration curve was appropriate for the analysis, as demonstrated by the accuracy, which was between 91.4% and 106.7%. Interday precision and accuracy on quality control samples at 9, 30 and 300 ng/ml were 3.1‐11.2% and 98.3–111.4%, respectively. The assay was applied successfully to determine the intratumor concentration of E‐3810 in different mouse xenograft tumor models and in a biopsy of a patient with breast cancer included in the phase I/II trial of the drug. In mouse tumors, the concentrations of E‐3810 were higher than necessary to exert antitumor activity in vitro (1 µM). Even more of interest was the result obtained in a human biopsy of few milligrams, where E‐3810 reached 4.9 µg/g (11 µM). Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
74.
Sala F Bagnati R Livi V Cereda R D'Incalci M Zucchetti M 《Journal of mass spectrometry : JMS》2011,46(10):1039-1045
E-3810, 6-[[7-[(1-aminocyclopropyl)methoxy]-6-methoxy-4-quinolyl]oxy]-N-methyl-naphthalene-1-carboxamide, is a novel, potent, dual inhibitor of vascular endothelial growth factor and fibroblast growth factor receptors with antiangiogenic properties, now under early clinical evaluation as an anticancer agent. To investigate its clinical pharmacokinetics, a high-performance liquid chromatography-tandem mass spectrometry method was developed and validated to measure the drug in human plasma on the basis of simple protein precipitation with methanol after addition of deuterated E-3810 as internal standard. The method requires a small volume of sample (100 μl) and is rapid and selective, allowing good resolution of peaks in 5 min. It is sensitive, precise, and accurate, with overall precision, expressed as CV%, always ≤7.1%, accuracy in the range 92.7%-104.4%, and high recovery, close to 100%. The limit of detection is 0.01 ng/ml, and the lower limit of quantitation is 2.0 ng/ml. The assay was validated in the range from the lower limit of quantitation up to 500.0 ng/ml. This is the first method developed and validated for analyzing E-3810 in human plasma. The method has been successfully applied to study E-3810 pharmacokinetics in cancer patients with solid tumors who are receiving daily oral doses of the drug during the phase I trial. 相似文献
75.
Delli Castelli D Terreno E Aime S 《Angewandte Chemie (International ed. in English)》2011,50(8):1798-1800
76.
Enzo Alessio Elisabetta Iengo Ennio Zangrando Silvano Geremia Patricia A. Marzilli Mario Calligaris 《欧洲无机化学杂志》2000,2000(10):2207-2219
77.
78.
Benincasa C Maiuolo L Mazzotti F Perri E Sindona G Urso E 《Journal of mass spectrometry : JMS》2004,39(1):61-65
A method is presented which allows the identification and assay of a nucleoside in the presence of other analogues and homologues. The method is based on the conventional multiple reaction monitoring approach performed on the [M + H]+ ions of wild-type and modified nucleosides produced by the turbo ionspray ionization method on a triple-quadrupole mass spectrometer. The accuracy of the quantitative determination relies on the evaluation of a response factor rho, which takes into account the kinetics of dissociation of the parent ions into the protonated [B + 2H]+ nucleobase ions. The evaluation of the absolute concentration of each analyte in the examined mixture does not require any previous chromatographic separation. 相似文献
79.
Schneider C Sreekanth AR Mai E 《Angewandte Chemie (International ed. in English)》2004,43(42):5691-5694
80.