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Purification Process of Total jiegumuglycosides
LU Qing-xiu,Yang Liu, Jiang Hai,Wang Qiu-hong,Yang Bing-you, Kuang Hai-xue*
Key Laboratory of Chinese Materia Medica, Heilongjiang University of Chinese Medicine, Ministry of Education,Key Laboratory of Traditional Chinese Medicine and Natural Medicine Pharmacodynamic Material Base,Harbin 150040, China
Abstract: Objective To investigate the optimum parameters to purify total jiegumu glycosides. Method morroniside as index components,was established by HPLC analysis method morroniside determination; purification on total jiegumu glycosides has been studied. Result The purification process of total jiegumu glycosides is as following: the flow rate is 1.5BV/h, and themacroporous adsorptive resins is AB-8, then abandon 20BV eluant, gather 10% alcohol holo-elution. Conclusion Purification process is simple, reliable, and suitable for industrial production.
Key words: Sambucus williamsii Hance; morroniside; purification process
Sambucus williamsii Hance has a long history of medicinal,only contained in the "Tang Materia Medica",its root and root bark, stems and leaves, flowers were for medicinal. Alone used to
splice joints solid odd, then used drugs in the blood and blood, and its role in bone optimal ......
"exposition [1] Accoarding to the preliminary studies of task Force [2,3],The root of jiegumu have significantly promote fracture healing, and to clarify the material basis for total jiegumu glycosides[4]. Because of the research group of Sambucus williamsii Hance extraction process were studied. From the experiments can be seen, the dry extract in ethanol extracts morroniside (active ingredient) content of about 13.5%, and in order to achieve an effective component accounted for 50% of the effective parts. In this paper, morroniside as reference for the purification of total jiegumu glucosides study.
Materials and methods 1.1 Materials
Waters-2695 high performance liquid chromatography; electronic analytical balance (Switzerland METTLER TOLEDO Company); HPD-750, HPD-600, HPD-100 macroporous resin (Changzhou Bao En adsorption material Technology Co., Ltd.); AB-8 , D3520, S-8 macroporous resin (Nankai University chemical Plant); morroniside reference: Heilongjiang University of Chinese Medicine Department of Chemistry homemade (purity 98%), experimental herbs collected from Heilongjiang Province, East County, the Heilongjiang Chinese Medicine University School of
Medicine and Chinese Medicine Resources Department Professor Wang Zhenyue identified as Sambucus williamsii Hance dried root bark.
1.2. Methods
1.2.1 The screening of resin type Weigh HPD-600, HPD-100, HPD-750, AB-8, D3520, S-8 resins 50g, column packing. Take 3g sample solution on the sample, water elution, per 100ml of outflow of fluid collect a times, measured the content of morroniside; The eluate of AB-8 resin morroniside out faster, and the recovery rate is high, Which ultimately determine the selection of AB-8 macroporous resin.
1.2..2 The screening test results and analysis of resin type HPD-750 resin:Water eluate was detected by HPLC, with a large number of polar compounds not meet the purpose of purification; S-8 resin:Morroniside together with a large number of polar compounds were eluted reach the separation effect, eliminate.HPD-600, D3520 two types of resins,Morroniside polar impurities can not be completely separated with the large, eliminate.AB-8 and HPD-100 can cause the large polar impurities morroniside with better separation.On the AB-8 and HPD-100 two models macroporous resin compare further found that:The peak area of AB-8 type resin elution peak area percentage greater than 80% of the eluent flow faster, and higher recovery rates, which ultimately determine the selection of AB-8 macroporous resin.
1.2.3 Determine the maximum amount of the sample Weigh four AB-8 macroporous resin 50g, water, wet packed column, numbered 1,2,3,4.Weigh 3g, 6g, 9g, 12g sample on the sample solution, eluted with water.Detect the presence of morroniside in eluate by TLC.Finally determine the maximum loading of about morroniside resin mass ratio of 1:250.
1.2.4 Determination of optimal elution flow rate Weigh four AB-8 macroporous resin 50g, water, wet packed column, numbered 1,2,3,4. Weigh the sample on the sample solution 3g, Respectively 1.0,1.5,2.0,2.5 BV / h flow rate of the water elution. Determination the content of morroniside, calculate recovery. Which 1.0BV / h, 1.5BV / h, 2.0BV / h, 2.5BV / h morroniside recoveries were 69.7%, 67.4%, 63.2%, 51.4%, Results: Macroporous resin column flow more slowly eluted, the better, but limit the slow eluting extend the production cycle, the production cost will increase. Therefore, considering choosing the best elution rate was 1.5BV / h.
1.2.5 Determination of optimum elution volume To determine the purification cycle, take six parts of AB-8 type macroporous resin column loading samples to 1.5BV / h flow rate, respectively, removal of 5,10,15,20,25,30 column volumes of wash water soluble impurities, then complete elution of 10% ethanol. Determination morroniside content,Calculate recovery.
Table 1 The yield of morroniside was influenced by water removal impurities
Category Water eluentBV The peak area of Morroniside Morroniside yield
1 5 76% 96%
2 10 81% 90%
3 15 91% 87%
4 20 92% 86%
5 25 80% 74%
6 30 73% 70%
(Note: The peak area percentage less than 80% of the mass percentage morroniside were less than 50%)
From Table 1, Eluted with solution No. 4, Available purity and yield are more impressive total jiegumu glycosides. Therefore, to determine elution with 20BV water-soluble impurities. Results and discussion
Experiment 3 batches, the results total jiegumu glycosides RSD was 0.653%, morroniside RSD was 1.5%. Thereby determining the optimum purification process Sambucus williamsii Hance.The most of the ethanol extract of Sambucus williamsii Hance polar impurities than morroniside, Use macroporous resin column is intended to be morroniside with these large polar impurities separation. This article on macroporous resin type, maximum sample volume, the best elution flow rate were screened. Conclusions
Best purification processes:In 1.5BV / h flow rate of water was eluted through the AB-8 type macroporous resin column chromatography, the water eluate discarded 20BV, collect 10% ethanol eluate was lyophilized to obtain total jiegumu glycosides.The three batches of validation tests showed that macroporous resin purification process stability, resulting elderberry total glucosinolate content of total glycosides (in morroniside meter) reached more than 51% recovery rate of 80% or more,This is the total jiegumu glucosides purification process. References
1. National Herbal Writing Group of the National Herbal Compendium (first volume) [M]. People's Health Press, 1975; 738.
2. Lu Fang. Thesis "elderberry chemical constituents of the root bark" Heilongjiang University of Chinese Medicine, 2002.
3. Han hua Elderberry root bark promote healing effective part of the chemical composition and pharmacological effects of Heilongjiang University of Chinese Medicine Doctoral Dissertation, 2006.
4. Han hua, Kuang Haixue, Li Zhenyu, etc. orthogonal test morroniside extraction process [J] Medicine Information, 2011,28 (4) :33-35.
Study on Preparation Technology of Total Jiegumu glycosides tablet
LU Qing-xiu,Yang Liu,Jiang Hai,Wang Qiu-hong,Yang Bing-you,Kuang Hai-xue*
Key Laboratory of Chinese Materia Medica,Heilongjiang University of Chinese Medicine,Ministry of Education,Key Laboratory of Traditional Chinese Medicine and Natural Medicine Pharmacodynamic Material Base,Harbin 150040, China
Abstract: Objective To establish the preparation of total jiegumu glycosides tablet . Method Using single factor method excipients were screened for the molding process studied for total jiegumu glycosides tablet.Result. Sambucus williamsii Hance
glycosides32g;lactose288g;MCC32g;PVPP7g;magnesiumstearate3.5g;Forming process is as following:fully combine the extract of total jiegumu glycosides and adjuvant as formula, and then filter the mixture, sieved, tabletting, ie.Conclusion Our group determine total jiegumu glycosides tablet that is the preparation technology scientific and stable .The chip can develop total jiegumu glycosides tablet and provide the basis for new drugs.
Key words: morroniside; total jiegumuglycosides tablet;preparation process
Sambucus williamsii Hance(jiegumu) known as hippurate show,big bone Dan and so on.Derived from Sambucus species of Caprifoliaceae[1].The main efficacies of jiugumu include fractures, bruises, swelling and bleeding trauma.The root of jiegumu have significantly promote fracture healing, and to clarify the material basis for total jiegumu glycosides.Task Force will total jiegumu glycosides prepared into tablets for clinical patients taking.Decoction is characterized oral dose, long home easily moldy. But there is an accurate dose tablets, stable quality, good
