Methotrexate （MTX） is an antineoplastic therapeutic medicine as antimetabolite of folic acid. In this paper, a sensitive and rapid ultra-performance liquid chromatographic （UPLC） method was developed and validated...Methotrexate （MTX） is an antineoplastic therapeutic medicine as antimetabolite of folic acid. In this paper, a sensitive and rapid ultra-performance liquid chromatographic （UPLC） method was developed and validated for the separation and determination of impurities in MTX drug substances. The UPLC method was accomplished on an Agilent Zorbax Extend C-18 （50 mm × 4.6 mm, 1.8 μm） with a gradient elution system composed of sodium dihydrogen phosphate in water （20 mmol/L, pH 3.0） and acetonitrile. The flow rate was 2.2 mL/min. The method was validated. The calibration curves displayed good linearity （r 〉 0.999） within the tested concentration ranges. The limit of detection （LOD） and limit of quantification （LOQ） of the six analytes were all less than 0.774 μg/mL and 1.03μg/mL. The relative standard deviation （RSD） for intra- and inter-day precision of the six analytes was less than 9.8%, including at the LOQ. The average recovery ranged from 95.2% to 103 except at the LOQ where recovery ranged from 82.7% to 117%. The validated method was successfully used to determine the relative abundance of six impurities in the MTX drug substances.展开更多
The novel justicidin G analogue 13 and its phosphate ester 15 were synthesized as potential anticancer agents in several steps starting from commercially available methyl gallate and veratraldehyde. The cytotoxicity o...The novel justicidin G analogue 13 and its phosphate ester 15 were synthesized as potential anticancer agents in several steps starting from commercially available methyl gallate and veratraldehyde. The cytotoxicity of the intermediates was tested against HCT-8, BEL-7402, KETR3, HELA, BGC-823, KB and MCF-7 cell lines by the MTT test, and compound 15 exhibited significant cytotoxicity in HELA and KB cell lines.展开更多
A novel and efficient approach for the straightforward synthesis of biologically significant acenaphtho[1,2-b]quinoline derivatives in good yields utilizing CuI as a catalyst with a broad array of substrates has been ...A novel and efficient approach for the straightforward synthesis of biologically significant acenaphtho[1,2-b]quinoline derivatives in good yields utilizing CuI as a catalyst with a broad array of substrates has been developed. The strategy features as a CuI-catalyzed cascade reaction involving the formation of two new C–C bonds and one new C–N bond with high atom economy. A proposed mechanism for the reaction is described.展开更多
基金Ministry of Public Health of the People’s Republic of China (No. 200802038)the Ministry of Science and Technology of the People’s Republic of China (No. 2011IM030200) for financial support of this work
文摘Methotrexate （MTX） is an antineoplastic therapeutic medicine as antimetabolite of folic acid. In this paper, a sensitive and rapid ultra-performance liquid chromatographic （UPLC） method was developed and validated for the separation and determination of impurities in MTX drug substances. The UPLC method was accomplished on an Agilent Zorbax Extend C-18 （50 mm × 4.6 mm, 1.8 μm） with a gradient elution system composed of sodium dihydrogen phosphate in water （20 mmol/L, pH 3.0） and acetonitrile. The flow rate was 2.2 mL/min. The method was validated. The calibration curves displayed good linearity （r 〉 0.999） within the tested concentration ranges. The limit of detection （LOD） and limit of quantification （LOQ） of the six analytes were all less than 0.774 μg/mL and 1.03μg/mL. The relative standard deviation （RSD） for intra- and inter-day precision of the six analytes was less than 9.8%, including at the LOQ. The average recovery ranged from 95.2% to 103 except at the LOQ where recovery ranged from 82.7% to 117%. The validated method was successfully used to determine the relative abundance of six impurities in the MTX drug substances.
基金National Major Scientific and Technological Special Project for ‘Significant New Drugs Innovation’ (No.2012ZX09301002001)the Union Youth Science&Research Fund(No.3332013074)
文摘The novel justicidin G analogue 13 and its phosphate ester 15 were synthesized as potential anticancer agents in several steps starting from commercially available methyl gallate and veratraldehyde. The cytotoxicity of the intermediates was tested against HCT-8, BEL-7402, KETR3, HELA, BGC-823, KB and MCF-7 cell lines by the MTT test, and compound 15 exhibited significant cytotoxicity in HELA and KB cell lines.
基金the National Key Technology R&D Program‘‘New Drug Innovation’’of China(No.2013ZX09402103)
文摘A novel and efficient approach for the straightforward synthesis of biologically significant acenaphtho[1,2-b]quinoline derivatives in good yields utilizing CuI as a catalyst with a broad array of substrates has been developed. The strategy features as a CuI-catalyzed cascade reaction involving the formation of two new C–C bonds and one new C–N bond with high atom economy. A proposed mechanism for the reaction is described.
