在Pirkle型的 (S ,S) Whelk O 1与纤维素衍生物型的CDMPC两种手性柱上对六种外消旋萘普生酯进行了对映体分离 ,通过研究烷氧基结构上的差异以及流动相中不同的醇类添加剂对手性识别的影响 ,探讨和比较了外消旋萘普生酯在两种手性固定...在Pirkle型的 (S ,S) Whelk O 1与纤维素衍生物型的CDMPC两种手性柱上对六种外消旋萘普生酯进行了对映体分离 ,通过研究烷氧基结构上的差异以及流动相中不同的醇类添加剂对手性识别的影响 ,探讨和比较了外消旋萘普生酯在两种手性固定相上手性识别的机理 .对于 (S ,S) Whelk O 1,溶质与固定相之间的吸引作用是手性识别的主要因素 ,而对于CDMPC 。展开更多
The cis and trans isomers separation of 2-butene-1,4-diol and lafutidine were studied by HPLC on two kinds of chiral columns: (S,S)-Whelk-O 1 and ChiraSpher. The isomers of 2-butene-1,4-diol can be separated on both c...The cis and trans isomers separation of 2-butene-1,4-diol and lafutidine were studied by HPLC on two kinds of chiral columns: (S,S)-Whelk-O 1 and ChiraSpher. The isomers of 2-butene-1,4-diol can be separated on both chiral columns while the isomers of lafutidine can only be resolved on ChiraSpher column. The influence of different type and amount of mobile phase modifier on the isomers separation was extensively studied. The resolution of cis and trans isomers of 2-butene-1,4-diol was 2.61on (S,S)-Whelk-O 1 column with hexane-ethanol (97:3, v/v) as the mobile phase. The resolution of lafutidine was 1.89 on ChiraSpher column with hexane-ethanol-THF-diethylamine (92:3:5:0.1, v/v/v/v) as the mobile phase. LC-MS methods were developed to identify the isomer peaks.展开更多
A selective, sensitive and high throughput liquid chromatography-tandem mass spectro-metry （LC-ESI-MS/MS） method has been developed for separation and quantification of metoprolol enantiomers on a chiral Lux Amylose...A selective, sensitive and high throughput liquid chromatography-tandem mass spectro-metry （LC-ESI-MS/MS） method has been developed for separation and quantification of metoprolol enantiomers on a chiral Lux Amylose-2 （250 mm＆#215;4.6 mm, 5 mm） column. Solid phase extraction of （S）-（-）- and （R）-（t）-metoprolol and rac-metoprolol-d6 as an internal standard （IS） was achieved on Lichrosep DVB HL cartridges employing 200 mL human plasma. Both the analytes were chromatographically separated with a resolution factor of 2.24 using 15 mM ammonium acetate in water, pH 5.0 and 0.1% （v/v） diethyl amine in acetonitrile （50：50, v/v） as the mobile phase within 7.0 min. The precursor-product ion transitions for the enantiomers and IS were monitored in the multiple reaction monitoring and positive ionization mode. The method was validated over the concentration range of 0.500-500 ng/mL for both the enantiomers. Matrix effect was assessed by post-column analyte infusion experiment and the mean extraction recovery was greater than 94.0% for both the enantiomers at all quality control levels. The stability of analytes was evaluated in plasma and whole blood under different storage conditions. The method was successfully applied to a clinical study in 14 healthy volunteers after oral administration of 200 mg metoprolol tablet under fasting conditions. The assay reproducibility is shown by reanalysis of 68 incurred samples. The suitability of the developed method was assessed in comparison with＆amp;nbsp;different chromatographic methods developed for stereoselective analysis of metoprolol in biological matrices.展开更多
(4S)-4-Carboxyl-1-oxoperoxovanatrane and (4S)-3-methyl-4-carboxyl-1-oxoperoxovanatrane were synthesized from the reaction of potassium vanadate. hydrogen peroxide with L-N, N-bis (2-hydroxyethyl) serine or L-N. N-bis ...(4S)-4-Carboxyl-1-oxoperoxovanatrane and (4S)-3-methyl-4-carboxyl-1-oxoperoxovanatrane were synthesized from the reaction of potassium vanadate. hydrogen peroxide with L-N, N-bis (2-hydroxyethyl) serine or L-N. N-bis (2-hydroxyethyl) threonine in water.展开更多
Chiral amino acids and their corresponding amino alcohols bearing camphoric backbone were prepared from D-（＋）-camphoric imide and characterized by infrared, elemental analysis, ESI-MS, and NMR measurements. Among t...Chiral amino acids and their corresponding amino alcohols bearing camphoric backbone were prepared from D-（＋）-camphoric imide and characterized by infrared, elemental analysis, ESI-MS, and NMR measurements. Among them, one intermediate （1S,3R）-3-amino-2,2,3- trimethyl cyclopentane-1-carboxylic acid hydrochloride 3 was structurally elucidated by X-ray diffraction techniques. Versatile intermolecular hydrogen bonding interactions observed in its packing structure result in a two-dimensional framework.展开更多
Chiral C2-symmetric N-heterocyclic carbene （NHC） palladium diaquo complex 5b prepared from （S）-BINAM was found to be a fairly effective catalyst for the enantioselective asymmetric fluorination of oxindoles to giv...Chiral C2-symmetric N-heterocyclic carbene （NHC） palladium diaquo complex 5b prepared from （S）-BINAM was found to be a fairly effective catalyst for the enantioselective asymmetric fluorination of oxindoles to give the corresponding products in moderate enantioselectivities along with good to excellent yields.展开更多
文摘在Pirkle型的 (S ,S) Whelk O 1与纤维素衍生物型的CDMPC两种手性柱上对六种外消旋萘普生酯进行了对映体分离 ,通过研究烷氧基结构上的差异以及流动相中不同的醇类添加剂对手性识别的影响 ,探讨和比较了外消旋萘普生酯在两种手性固定相上手性识别的机理 .对于 (S ,S) Whelk O 1,溶质与固定相之间的吸引作用是手性识别的主要因素 ,而对于CDMPC 。
文摘The cis and trans isomers separation of 2-butene-1,4-diol and lafutidine were studied by HPLC on two kinds of chiral columns: (S,S)-Whelk-O 1 and ChiraSpher. The isomers of 2-butene-1,4-diol can be separated on both chiral columns while the isomers of lafutidine can only be resolved on ChiraSpher column. The influence of different type and amount of mobile phase modifier on the isomers separation was extensively studied. The resolution of cis and trans isomers of 2-butene-1,4-diol was 2.61on (S,S)-Whelk-O 1 column with hexane-ethanol (97:3, v/v) as the mobile phase. The resolution of lafutidine was 1.89 on ChiraSpher column with hexane-ethanol-THF-diethylamine (92:3:5:0.1, v/v/v/v) as the mobile phase. LC-MS methods were developed to identify the isomer peaks.
文摘A selective, sensitive and high throughput liquid chromatography-tandem mass spectro-metry （LC-ESI-MS/MS） method has been developed for separation and quantification of metoprolol enantiomers on a chiral Lux Amylose-2 （250 mm＆#215;4.6 mm, 5 mm） column. Solid phase extraction of （S）-（-）- and （R）-（t）-metoprolol and rac-metoprolol-d6 as an internal standard （IS） was achieved on Lichrosep DVB HL cartridges employing 200 mL human plasma. Both the analytes were chromatographically separated with a resolution factor of 2.24 using 15 mM ammonium acetate in water, pH 5.0 and 0.1% （v/v） diethyl amine in acetonitrile （50：50, v/v） as the mobile phase within 7.0 min. The precursor-product ion transitions for the enantiomers and IS were monitored in the multiple reaction monitoring and positive ionization mode. The method was validated over the concentration range of 0.500-500 ng/mL for both the enantiomers. Matrix effect was assessed by post-column analyte infusion experiment and the mean extraction recovery was greater than 94.0% for both the enantiomers at all quality control levels. The stability of analytes was evaluated in plasma and whole blood under different storage conditions. The method was successfully applied to a clinical study in 14 healthy volunteers after oral administration of 200 mg metoprolol tablet under fasting conditions. The assay reproducibility is shown by reanalysis of 68 incurred samples. The suitability of the developed method was assessed in comparison with＆amp;nbsp;different chromatographic methods developed for stereoselective analysis of metoprolol in biological matrices.
文摘(4S)-4-Carboxyl-1-oxoperoxovanatrane and (4S)-3-methyl-4-carboxyl-1-oxoperoxovanatrane were synthesized from the reaction of potassium vanadate. hydrogen peroxide with L-N, N-bis (2-hydroxyethyl) serine or L-N. N-bis (2-hydroxyethyl) threonine in water.
基金This work was funded by the National Natural Science Foundation of China (No. 20301009)
文摘Chiral amino acids and their corresponding amino alcohols bearing camphoric backbone were prepared from D-（＋）-camphoric imide and characterized by infrared, elemental analysis, ESI-MS, and NMR measurements. Among them, one intermediate （1S,3R）-3-amino-2,2,3- trimethyl cyclopentane-1-carboxylic acid hydrochloride 3 was structurally elucidated by X-ray diffraction techniques. Versatile intermolecular hydrogen bonding interactions observed in its packing structure result in a two-dimensional framework.
文摘Chiral C2-symmetric N-heterocyclic carbene （NHC） palladium diaquo complex 5b prepared from （S）-BINAM was found to be a fairly effective catalyst for the enantioselective asymmetric fluorination of oxindoles to give the corresponding products in moderate enantioselectivities along with good to excellent yields.
