建立了一种简捷、快速测定L-高丝氨酸内酯盐酸盐的分析方法,L-高丝氨酸内酯盐酸盐经氯甲酸笏甲酯(FMOC-Cl)衍生化后用HPLC定量分析。采用Wonda Sil C18色谱柱,流动相为乙腈-水(体积比为50∶50),流量为1.0m L/min,柱温为25℃,检测波长为2...建立了一种简捷、快速测定L-高丝氨酸内酯盐酸盐的分析方法,L-高丝氨酸内酯盐酸盐经氯甲酸笏甲酯(FMOC-Cl)衍生化后用HPLC定量分析。采用Wonda Sil C18色谱柱,流动相为乙腈-水(体积比为50∶50),流量为1.0m L/min,柱温为25℃,检测波长为210nm进行检测。该方法的线性相关系数为0.9991,标准偏差为0.0016,平均回收率为99.39%。展开更多
A solid phase derivatization method of amino acids and peptides was described. Samples were added on alkaline silica gel cartridge and dried. The derivatization was carried out by passing the derivatization regent dis...A solid phase derivatization method of amino acids and peptides was described. Samples were added on alkaline silica gel cartridge and dried. The derivatization was carried out by passing the derivatization regent dissolved in anhydrous solvent through the cartridge slowly, then the cartridge was washed with a selected solvent, finally, the derivatives were eluted. The eluates were separated and detected by means of HPLC with fluorescence detector. Three derivatization reagents, 9\|fluorenylmethyl chloroformate(FMOC\|Cl), \{7\|chloro\|4\|nitrobenzo\|2\|oxa\|1,3\|diazole\}(NBD\|Cl) and fluorescein isothiocyanate(FITC) were investigated with this method. The results showed that the method was suitable for derivatization of amino acids and some of peptides with FMOC\|Cl because of its highly reacting activity and low polarity, the side\|products of the FMOC\|Cl with water were greatly decreased, the excess FMOC\|Cl was eliminated completely, and the silica gel support did not significantly affect the reaction rate and yield for amino acids. NBD\|Cl was not suitable for this method because of the low yield of derivatization. FITC was also not suitable for this method because of its strong polarity.展开更多
建立并优化了高效液相色谱测定草铵膦含量的检测方法。在碱性条件下草铵膦与氯甲酸-9-芴基甲酯(FMOC-CL)反应,对衍生物进行液相色谱分离和测定,以乙腈、甲醇、磷酸水溶液作为流动相,使用Diamonsil Plus 5μm C18柱为分离柱,在206nm波长...建立并优化了高效液相色谱测定草铵膦含量的检测方法。在碱性条件下草铵膦与氯甲酸-9-芴基甲酯(FMOC-CL)反应,对衍生物进行液相色谱分离和测定,以乙腈、甲醇、磷酸水溶液作为流动相,使用Diamonsil Plus 5μm C18柱为分离柱,在206nm波长下检测。本方法衍生反应时间快,有效成分与杂质能够得到很好的分离,衍生产物稳定。三个样品的加标回收率分别为99.93%、99.61%、99.39%;相对标准偏差分别为0.03、0.02、0.03;变异系数分别为0.17%、0.09%、0.02%。本方法使用C18柱较耐用,检测灵敏度高,适用于各种草铵膦微量以及痕量的样品检测。展开更多
文摘建立了一种简捷、快速测定L-高丝氨酸内酯盐酸盐的分析方法,L-高丝氨酸内酯盐酸盐经氯甲酸笏甲酯(FMOC-Cl)衍生化后用HPLC定量分析。采用Wonda Sil C18色谱柱,流动相为乙腈-水(体积比为50∶50),流量为1.0m L/min,柱温为25℃,检测波长为210nm进行检测。该方法的线性相关系数为0.9991,标准偏差为0.0016,平均回收率为99.39%。
文摘A solid phase derivatization method of amino acids and peptides was described. Samples were added on alkaline silica gel cartridge and dried. The derivatization was carried out by passing the derivatization regent dissolved in anhydrous solvent through the cartridge slowly, then the cartridge was washed with a selected solvent, finally, the derivatives were eluted. The eluates were separated and detected by means of HPLC with fluorescence detector. Three derivatization reagents, 9\|fluorenylmethyl chloroformate(FMOC\|Cl), \{7\|chloro\|4\|nitrobenzo\|2\|oxa\|1,3\|diazole\}(NBD\|Cl) and fluorescein isothiocyanate(FITC) were investigated with this method. The results showed that the method was suitable for derivatization of amino acids and some of peptides with FMOC\|Cl because of its highly reacting activity and low polarity, the side\|products of the FMOC\|Cl with water were greatly decreased, the excess FMOC\|Cl was eliminated completely, and the silica gel support did not significantly affect the reaction rate and yield for amino acids. NBD\|Cl was not suitable for this method because of the low yield of derivatization. FITC was also not suitable for this method because of its strong polarity.
文摘建立并优化了高效液相色谱测定草铵膦含量的检测方法。在碱性条件下草铵膦与氯甲酸-9-芴基甲酯(FMOC-CL)反应,对衍生物进行液相色谱分离和测定,以乙腈、甲醇、磷酸水溶液作为流动相,使用Diamonsil Plus 5μm C18柱为分离柱,在206nm波长下检测。本方法衍生反应时间快,有效成分与杂质能够得到很好的分离,衍生产物稳定。三个样品的加标回收率分别为99.93%、99.61%、99.39%;相对标准偏差分别为0.03、0.02、0.03;变异系数分别为0.17%、0.09%、0.02%。本方法使用C18柱较耐用,检测灵敏度高,适用于各种草铵膦微量以及痕量的样品检测。