| Radix Ophiopogon was the root of Liliaceae Ophiopogon japonicas(L.f)K.er-Gawl.Currently the market divided Ophiopogon japomicas(L.f)Ker-Gawl. into Zhe jiang Radix Ophiopogon, and sichuan Radix Ophiopogon base on origin, there gr owth years and Characters are different. Zhejiang Radix Ophiopogon growth of three to four years after the excavation as herbs, sichuan Radix Ophiopogon growth o ne year after the excavation as herbs. Quality traditionally considered the best in Zhejiang, but at present the largest production in Sichuan. Zhejiang Radix Ophi opogon is one of the famous "Zhejiang Bawei",and the quality of Zhejiang Rad ix Ophiopogon is excellent, but no systematic comparison on the Zhejiang Radi x Ophiopogon and sichuan Radix Ophiopogon ingredients reported. Radix Ophio pogon were contained in the2010version of "Chinese Pharmacopoeia" traits an d microscopic identification, TLC. and total saponin content determination, it had not been able to systematically analyze the quality of Radix Ophiopogon. Shen mai injection which produced in chiatal qingchun bao pharmaceutical co.,Itd.Zheji ang Radix Ophiopogon used zhejiang Radix Ophiopogon as raw material, so we also studied its content. We mostly study the Zhejiang Radix Ophiopogon,usi ng the modern analytical techniques, we establish a quality control method to ev aluate and control the quality of Ophiopogon japonicas(L.f)Ker-Gawl.tecomprehen sively through the research of chemical composition, fingerprints, qualitative iden tification and quantitative analysisObjective:(1) to study the chemical composition of Zhejiang Radix Ophiopogo n and sichuan Radix Ophiopogon, finding the distinguished characteristic ingredi ents of them.(2) to establish the high performance liquid chromatography (HPL C) fingerprint method of Flavonoids in Ophiopogon japonicas(L.f)Ker-Gawl., Com parison of the similarities and differences between Ophiopogon japonicus from zhejiang and sichuan.(3) to establish the quantitative analytical method of flavo noids in Ophiopogon japonicas(L.f)Ker-Gawl.。(4) to study the Characters between Ophiopogon japonicus from zhejiang and sichuan and to establish the thin layer chromatography (TLC) methods for distinguishing Ophiopogon japonicus from zhej iang and sichuan (5) to study the change of content in different hardvest times a nd different processing methods.(6) to establish the quantitative analytical method in shenmai InjectionMethods:(1) study the chemical composition between Ophiopogon japonicus fr om zhejiang and sichuan。Identified and analyzed the Volatile components by GC-MS; separated and identified the characteristic components in Ophiopogon japonicas(L. f)Ker-Gawl. by the means of ODS column chromatography,silicagel column chro matography,preparation HPLC methods,etc.(2) Established the fingerprint of the characteristic components in Ophiopogon japonicas(L.f)Ker-Gawl.with the method o f HPLC, and then the method validation was studied.(3) HPLC method was use d to determine simultaneously in Ophiopogon japonicas(L.f)Ker-Gawl. and the m ethod validation was then studied.(4) Distingushing Ophiopogon japonicus from z hejiang and sichuan by Character identifying and microscopic identifying. Establi shed the TLC methods to Distingush Ophiopogon japonicus from zhejiang and sichuan(5) Studied determination and analyzed the contents of different harvest ti mes and processing methods.(6) HPLC method was used to determine simultaneo usly in shenmai injection and the method validation was then studied.Results:(1) I Zhejiang Radix Ophiopogonis and Sichuan Radix Ophiopogonis h ave certain differences in volatile composition. Zhejiang Radix Ophiopogonis was detected14peaks, but Sichuan Radix Ophiopogonis was only detected6peaks through GC-MS detection analysis. Both have two common peaks, besides, Zhe jiang Radix Ophiopogonis is higher in the content. Ⅱ Zhejiang Radix Ophiopogoni s and Sichuan Radix Ophiopogonis have some differences in flavonoids. Zhejian g Radix Ophiopogonis has four characteristic components which can be distingui shed from Ophiopogon japonicus. The content of6-aldehyde-7-methoxy isobut yl Ophiopogon flavanone B and Ophiopogonanone D of Zhejiang Radix Ophiopo gonis were higher, while the content of them was very low or even failed to be detect in Sichuan Radix Ophiopogonis.But the two chemicals are both found in Zhejiang Radix Ophiopogonis and Sichuan Radix Ophiopogonis. The unique fla vonoid features in Radix Ophiopogonis were extracted and separated. Besides we used NMR obtaining the6-aldehyde-7-methoxy isobutyl Ophiopogon flavano ne B and Ophiopogonanone D. Through reference substances verification, LC-M S and Spectral comparison of HPLC, we confirmed the common ingredients of Zhejiang Radix Ophiopogonis and Sichuan Radix Ophiopogonis were Methyloph iopogonanone A Methylophiopogonanone B, but but the proportion of the two i ngredients were different. ⅢThrough the study of Zhejiang Radix Ophiopogonis and Sichuan Radix Ophiopogonis n-butanol part,overall,the n-butanol part had li ttle difference. Zhejiang Radix Ophiopogonis contained borneol glycoside.while th e ingredient was not detected in Sichuan Radix Ophiopogonis.And saponin D is very low in Zhejiang Radix Ophiopogonis.but it was higher in comparison wit h Sichuan Radix Ophiopogonis.(2)We established the method of HPLC fingerpri nt of Zhejiang Radix Ophiopogonis and Sichuan Radix Ophiopogonis flavonoids.t hey all have8peaks, their similarities were all greater than0.9. But in Radix Ophiopogonis fingerprints to determination of Ophiopogon japonicus samples,10batches of Ophiopogon japonicus sample similarity were lower than0.8, both h ave great difference in composition. If we determinated the Ophiopogon japonicu s samples based on Radix Ophiopogonis fingerprints.10batches of Ophiopogon japonicus samples similarities were lower than0.8which showed that both had great differences.(3) I A HPLC method was built to determinated Methylophiopog onanone A Methylophiopogonanone B in dwarf lilyturf root simultaneously. Af ter verification methodology, The average recovery were102.9%(RSD=2.6%)、98.7%(RSD=2.0%) respectively, the linear, repeatability,stability were satisfactory. By determinating10batches of Radix Ophiopogonis and Ophiopogon japonicus samples, we found that content of the two ingredients in Radix Ophiopogonis is higher than that in Ophiopogon japonicus, the proportion of them is different. Ⅱ. UV spectrophotometer was established to determine total flavonoids in Ophiopo gon japonicus from zhejiang and sichuan. linearityn repeatability experiments、Sta bility, durability met the requirements.6batches the Zhejiang Radix and Chuanma i of winter each sample determination, the result showed Ophiopogon japonicus from zhejiang’s centent was higher.Ⅲ. simultaneous determination of were estab lished with the method HPLC in Ophiopogon japonicas(L.f)Ker-Gawl.. the resul ts of the method validation study showed that the average recovery were102.9%(RSD=2.6%),linearity、repeatability experiments、Stability, durability met the req uirements. Ⅳ. Ophiopogonin D levels were measured in Ophiopogon japonicus from zhejiang and sichuan. the results shows were very low, and Ophiopogon j aponicus from sichuan were slightly higher. V. The method for the determination of the samples with Ophiopogon japonicus from zhejiang and sichuan the total saponins under the2010version of "Chinese Pharmacopoeia", the result was not significantly different.(4) there have Certain distinction of Characters and microsco pic identification in Ophiopogon japonicus from zhejiang and sichuan, their shap e and odor both have Certain difference, the thin layer chromatography (TLC) metho ds was established to identify Ophiopogon japonicus from zhejiang and sichuan,t he result of the Rf were clear and specific.(5) Ⅰ.simultaneous determination of Methylophiopogonanone A and Methylophiopogonanone B in Ophiopogon japonic as(L.f)Ker-Gawl. collected from different harvest times and processing methods were established with the mehord HPLC. the results showed Methylophiopogona none A and Methylophiopogonanone B have trends in different harvest times wit h the change of time,but different processing methods have little change. Ⅱ. Diff erent harvest times and processing methods of total flavonoids were determined the result showed the content of different harvest times increased gradually with the changing time.but the content of differentprocessing methods have little ch ange.Ⅲ. establishing method for the determination of in different harvest season s and processing methods,the result showed the content have little change fro m Match to June and it has increased gradually from July to September,but the content of different processing methods have little change. Ⅳ. The method for th e determination of the samples with different harvesting time the total saponins under the2010version of "Chinese Pharmacopoeia", the result was not significa ntly different.(6) simultaneous determination of were established with the metho d HPLC in shenmai injection, the results of the method validation study showed that the average recovery were98.7%(RSD=2.0%).linearity、repeatability experi ments、Stability, durability met the requirements.Conclution:(1) The subject according to compare the compositions between Ophiopogon ja ponicus from zhejiang and sichuan, the characteristic composition to distinguish Ophiopogon japonicus from zhejiang and Sichuan was clear, it can provide the i nspection index for the quality control of Ophiopogon japonicas(L.f)Ker-Gawl. an d further exploration study for the activity ingredient offering its material base.(2) It provide the methods to control the quality of Ophiopogon japonicus from zhej iang and Sichuan by establishing the method of fingerprint.(3) it provide the m ethods to control the quality of Ophiopogon japonicas(L.f)Ker-Gawl.to achieve st able and controllable by establishing the methods of hplc determination and TLC.(4) the difference of characters and microscopic identification between Ophiopog on japonicus from zhejiang and sichuan was clear, which could provide the bas is for varieties identification, and help to control the quality of Ophiopogon japo nicas(L.f)Ker-Gawl..(5) by researching the characteristic composition content of Ophiopogon japonicas(L.f)Ker-Gawl. in different time of harvest and different pr ocessing methods, we clear the content trends. it can provide the famous-region drug detection index for the quality control of Ophiopogon japonicas(L.f)Ker-Ga wl., it’s helpful to promote the development and utilization of Ophiopogon japon icas(L.f)Ker-Gawl..(6) the quality standards of shenmai injection will improve b y establishing the determination analytical method for determination of.it will al so help to control the stability of the production and ensure the security and sta bility of the production, in addition, it will be a significance for guiding and c ontrolling the actual production processes... |
PDF Full Text Request