为了建立分离度好、分离效率高的叶黄素顺、反异构体检测方法。通过对检测波长、流动相、流动相比例和流速等色谱条件的摸索和优化,确定最佳色谱条件,并采用光谱、高效液相色谱、质谱等方法对叶黄素顺、反异构体进行定性定量分析。结果...为了建立分离度好、分离效率高的叶黄素顺、反异构体检测方法。通过对检测波长、流动相、流动相比例和流速等色谱条件的摸索和优化,确定最佳色谱条件,并采用光谱、高效液相色谱、质谱等方法对叶黄素顺、反异构体进行定性定量分析。结果表明：该方法流动相为二氯甲烷-乙腈-甲醇（20∶30∶50,V/V）,流速为1.0 m L/min,叶黄素热异构化样品中各物质在12 min内达到有效分离,无拖尾现象,峰形较好;在叶黄素热异构化样品中鉴定出15-顺式、13/13′-顺式和9/9′-顺式叶黄素顺式异构体及全反式叶黄素,全反式叶黄素在4-260 ng范围内峰面积与进样量呈良好线形性关系,回收率在95%以上,精密度和稳定性相对标准偏差均小于2%。该方法分离度好、准确性高、重现性好。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
文摘为了建立分离度好、分离效率高的叶黄素顺、反异构体检测方法。通过对检测波长、流动相、流动相比例和流速等色谱条件的摸索和优化,确定最佳色谱条件,并采用光谱、高效液相色谱、质谱等方法对叶黄素顺、反异构体进行定性定量分析。结果表明：该方法流动相为二氯甲烷-乙腈-甲醇（20∶30∶50,V/V）,流速为1.0 m L/min,叶黄素热异构化样品中各物质在12 min内达到有效分离,无拖尾现象,峰形较好;在叶黄素热异构化样品中鉴定出15-顺式、13/13′-顺式和9/9′-顺式叶黄素顺式异构体及全反式叶黄素,全反式叶黄素在4-260 ng范围内峰面积与进样量呈良好线形性关系,回收率在95%以上,精密度和稳定性相对标准偏差均小于2%。该方法分离度好、准确性高、重现性好。
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.
