| In order to effectively control th e quality of Cortex Periplocae and provide reference for clinical application, in the study, On the basis of research on the chemical constituents, multiple components in Cortex Periplocae and its preparation were researched.1.To study the chemical constituents of Cortex Periplocae,separated and purified the ethanol(70％)extract of Cortex Periplocae by using many chromatographic methods and fourteen compounds were isolated and identified as 21-O-methyl-△5-pregnene-3β,14β,17β,21-tetraol-20-one-3-O-β-D-oleandropyranosyl(1'4)-β-D-cymaropyranosyl-(1'4)-β-D-cymaropyrano-syl(1),2-hydroxy-5-(2一hydroxy-4-methoxybenzyl)-4-methoxybenzaldehy-de(2),periplocoside M(3),△5-pregnene-3β,16β,20(R)-triol-20-O-β-Dglu-copyranosyl-(1'6)-β-D-glucopyranosyl-(1'2)-β-D-digitalopyranoside(4), △5-pregnene-3β,16α,20(S)-triol-20-O-β-D-glucopyranosyl-(1'6)-β-D-gluco-pyranosyl-(1'2)-β-D-digitalopyranoside(5),△5-pregnene-3β,20(S)-diol-20-O-β-D-glucopyranosyl-(1'6)-β-D-glucoyranosyl(1'2)-β-D-digitalopyranos-ide(6),glycoside H2(7),21-O-methyl-△5-pregnene-3β,14β,17β,20-tetraol (8),21-D-methyl-△5-pregnene-3β,14β,17β,21-tetraol-20-one(9),S-I(10), △5-pregnene-3β,16α,20α-triol(11),△5-pregnene-3β,17α,20α-trin(12),S-5A (13),S-2A(14)by using spectroscopic techniques including UV.IR. HR-MS、1H-NMR、13C-NMR.HMBC and HMQC.Amngg them,compound 1 is a new one and compound 3-14 are all C21 steroidals.2.A rapid,efficient and sensitive method using ultra-high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was developed for simultaneous determination of 7 components in Cortex Periplocae. Chromatographic separation was performed on a Waters AQUITY UPLC BEH C18 column using a gradient elution program with acidified aqueous and acetonitrile.Detection and quantitation were ac complished by a triple quadrupole mass spectrometer using multiple reaction-monitoring(MRM) scanning. The precursor and product ions of the analytes were monitored in positive and negative mode at the same time. The seven analytes:△5-pregnene-3/β,16β,20(R)-triol-20-O-β-D-glucopyranosyl-(1'6)-β-D-glucopyranosyl-(1'2)-D-digitalopyranoside (compound 1), periplocoside(compound 2), △5-pregnene-3β,16α,20(S)-triol-20-O-β-D-glucopyranosyl-(1'6)-β-D-glucopyranosyl-(1'2)-D-digitalopyra-noside(compound 3), periplocaglycoside H?(compound 4), periploca glycoside H](compound 5), periplocoside M(compound 6), periplocoside P(compound 7) showed good linearity (R2>0.9947) within the test range, the average recoveries were 98.11～102.86%, and the RSD were all less than 2.49%, respectively. The established method is simple, rapid and accurate and was successfully applied to investigate 26 batches of Cortex Periplocae from different source, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were employed to differentiate and classify the samples. The results indicated that there was certain correlation between the content of 7 ingredients in Cortex Periplocae and their sources, the method was useful not only for chemotaxonomy of numerous samples from different regions but also for standardization and differentiation of many similar samples.3. To establish an UPLC-MS method for determination of twelve compounds in qiliqiangxin capsμLes, the chromatographic separations were performed on a C18 column with gradient elution of acetonitrile and 0.1% aqueous formic acid. The monitoring of all analytes was achieved under the negative ionization mode. The twelve analytes showed good linearity (r2>0.9990) within the test ranges, the average recoveries were 98.20%-101.83%, respectively, the RSD were less than 3.88%, respectively. The established method was accurate and reliable can be used for quality control of qiliqiangxin capsμLes. |
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