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
基金Science Faculty Strategic Research of Hong Kong Baptist University(FRG/03-04/Ⅱ-51)中国科学院知识创新工程"集约化养殖场畜禽粪便的农用风险与污染控制"(kzcx3-sw-435)江苏省自然科学基金前期预研项目(BK2004219)资助
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.
