Morroniside consists of two anomeric isomers, α-morroniside and β-morroniside. These two anomeric compounds have been separated by reversed-phase high-performance liquid chromatography(HPLC) using a gradient mobile ...Morroniside consists of two anomeric isomers, α-morroniside and β-morroniside. These two anomeric compounds have been separated by reversed-phase high-performance liquid chromatography(HPLC) using a gradient mobile phase of acetonitrile-water at 7 ℃, and verified to be anomers of morroniside by ESI-TOF-MS. The higher peak in the chromatogram was appointed to α-morroniside according to NMR data reported in previous literature. The molar ratio of α-morroniside to β-morroniside was found to be 2.855∶1 at 25 ℃. Temperature appeared to be an important factor, which affects the separation result, and a better separation was achieved at a lower temperature. The relative peak height of β-morroniside in the total ion current chromatogram measured with positive ion ESI-TOF mass spectrometer was only a half of that in UV chromatogram. This indicates that β-morroniside is less sensitive to positive ion electrospray ionization than the α-isomer.展开更多
In this work six kinds of tartrate diesters were prepared from D(-), L(+) or DL-tartaric acid respectively, and their structure were verified by IR and NMR. The extraction behavior of optical compounds, D(-) ephedrine...In this work six kinds of tartrate diesters were prepared from D(-), L(+) or DL-tartaric acid respectively, and their structure were verified by IR and NMR. The extraction behavior of optical compounds, D(-) ephedrine and L(+) pseudoephedrine, was investigated at room temperature using prepared tartrate diester as extracting agent and n -heptane as diluent. The ratio of tartrate diester and n -heptane is 1∶1. Distribution coefficients, obtained from experiment data by material balance, show that there is a chiral recognition: L(+) tartrate diesters favour extraction of L(+) pseudoephedrine,while D(-) tartrate diesters favour extraction of D(-) ephedrine. The extraction behavior of the mixture of the above optical active epimerides, was also investigated under the same experimental conditions. The experiment data with HPLC also showed the same conclusion. Meanwhile, a blank experiment was carried out and the result showed that there was no evident effect on extraction distribution coefficients when extraction process occurred in the presence of n -heptane. The relationship between the structure of extracting agent and optical activity of the epimerides was also discussed.展开更多
以γ-环糊精和D-苯丙氨酸为手性选择剂,采用毛细管区带电泳成功地分离了新型抗菌素西他沙星差向异构体。考察了添加剂的种类、浓度和缓冲溶液的pH对毛细管电泳分离西他沙星的影响。分离电压为15kV,选用60cm(有效长度52.5cm)×50μm ...以γ-环糊精和D-苯丙氨酸为手性选择剂,采用毛细管区带电泳成功地分离了新型抗菌素西他沙星差向异构体。考察了添加剂的种类、浓度和缓冲溶液的pH对毛细管电泳分离西他沙星的影响。分离电压为15kV,选用60cm(有效长度52.5cm)×50μm i.d.的石英毛细管,缓冲溶液组成为10mm o l/L KH2PO4-K2HPO4(pH4.5),10mm o l/L C uSO4,20mm o l/Lγ-环糊精和10mm o l/LD-苯丙氨酸。实验结果表明,添加剂的种类和浓度是影响西他沙星手性分离的重要因素,只有当D-苯丙氨酸、铜离子和γ-环糊精同时存在并达到一定浓度时,西他沙星差向异构体在毛细管电泳中才具有良好的分离效果。该方法可用于西他沙星差向异构体的定量分析。展开更多
文摘Morroniside consists of two anomeric isomers, α-morroniside and β-morroniside. These two anomeric compounds have been separated by reversed-phase high-performance liquid chromatography(HPLC) using a gradient mobile phase of acetonitrile-water at 7 ℃, and verified to be anomers of morroniside by ESI-TOF-MS. The higher peak in the chromatogram was appointed to α-morroniside according to NMR data reported in previous literature. The molar ratio of α-morroniside to β-morroniside was found to be 2.855∶1 at 25 ℃. Temperature appeared to be an important factor, which affects the separation result, and a better separation was achieved at a lower temperature. The relative peak height of β-morroniside in the total ion current chromatogram measured with positive ion ESI-TOF mass spectrometer was only a half of that in UV chromatogram. This indicates that β-morroniside is less sensitive to positive ion electrospray ionization than the α-isomer.
文摘In this work six kinds of tartrate diesters were prepared from D(-), L(+) or DL-tartaric acid respectively, and their structure were verified by IR and NMR. The extraction behavior of optical compounds, D(-) ephedrine and L(+) pseudoephedrine, was investigated at room temperature using prepared tartrate diester as extracting agent and n -heptane as diluent. The ratio of tartrate diester and n -heptane is 1∶1. Distribution coefficients, obtained from experiment data by material balance, show that there is a chiral recognition: L(+) tartrate diesters favour extraction of L(+) pseudoephedrine,while D(-) tartrate diesters favour extraction of D(-) ephedrine. The extraction behavior of the mixture of the above optical active epimerides, was also investigated under the same experimental conditions. The experiment data with HPLC also showed the same conclusion. Meanwhile, a blank experiment was carried out and the result showed that there was no evident effect on extraction distribution coefficients when extraction process occurred in the presence of n -heptane. The relationship between the structure of extracting agent and optical activity of the epimerides was also discussed.
文摘以γ-环糊精和D-苯丙氨酸为手性选择剂,采用毛细管区带电泳成功地分离了新型抗菌素西他沙星差向异构体。考察了添加剂的种类、浓度和缓冲溶液的pH对毛细管电泳分离西他沙星的影响。分离电压为15kV,选用60cm(有效长度52.5cm)×50μm i.d.的石英毛细管,缓冲溶液组成为10mm o l/L KH2PO4-K2HPO4(pH4.5),10mm o l/L C uSO4,20mm o l/Lγ-环糊精和10mm o l/LD-苯丙氨酸。实验结果表明,添加剂的种类和浓度是影响西他沙星手性分离的重要因素,只有当D-苯丙氨酸、铜离子和γ-环糊精同时存在并达到一定浓度时,西他沙星差向异构体在毛细管电泳中才具有良好的分离效果。该方法可用于西他沙星差向异构体的定量分析。
