CN101838341A - Method for extracting polysaccharide from limonium sinense kuntze - Google Patents
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Abstract
本发明涉及天然药物领域，具体公开了一种中华补血草多糖的提取方法。其特征是用下列方法制得：将中华补血草全根干燥，粉碎，用蒸馏水提取1～3次，合并提取液，浓缩、乙醇沉淀、取沉淀物冷冻干燥，即得，其中提取温度为90℃～100℃，水浴提取之前超声，超声时间为40min～60min。本发明在常规多糖提取的工艺上进行优化，提取得到的中华补血草多糖的提取率达到12.80％。The invention relates to the field of natural medicines, and specifically discloses a method for extracting polysaccharides from Limonium sinensis. It is characterized in that it is obtained by the following method: dry the whole root of Limonium sinensis, crush it, extract it with distilled water for 1 to 3 times, combine the extracts, concentrate, precipitate with ethanol, and freeze-dry the precipitate to obtain it. The extraction temperature is 90 ℃～100℃, ultrasonication before water bath extraction, the ultrasonication time is 40min～60min. The invention optimizes the conventional polysaccharide extraction process, and the extraction rate of the Limonium sinensis polysaccharide can reach 12.80%.
Description
Technical field
The present invention relates to natural medicine field, specifically disclose a kind of optimization extraction process of limonium sinenseKuntze polysaccharide.
Background technology
Limonium sinenseKuntze (Limonium sinense (Girard) Kuntze), have another name called Root of Chinese Sealavender, salt cloud grass, the sea spinach, the sea radix paeoniae rubrathe etc., secrete the salt herbaceous plant for Statice (Limonium Mill.) is perennial, happiness is born on the coastal saliferous low-level bog, be distributed in northeast, North China, northwest and Tibet and coastal provinces district, mainly be distributed in Lianyun Harbour, northern Suzhou in Jiangsu, the Guanyun, the shining sun, East Platform, as east, (Chen Xinglong on the beach and saline-alkali wetland of coastlands such as Nantong, An Shuqing, Li Guoqi, Deng. Chinese littoral zone salt tolerant economic plants resource. Nanjing Forestry University's journal, 1999,23 (4): 81-84; Guo Qiaosheng, Su Xiaojuan. wild medicinal plant species diversity of the coastal beach in Jiangsu Province and protection thereof. Chinese wild plant resource, 1999,18 (3); 28-30).Except that having effects such as higher ornamental value and environment protection, folklore uses its treatment some diseases.
Existing discovering, this plant chemical ingredient is very abundant, contain multiple composition (Lin LC such as amino acid, inorganic elements, VITAMIN, flavonoid, tannin, polysaccharide, alkaloid, organic acid, Chou CJ.Flavonoids and phenolics fromLimonium sinense.Planta Med.2000,, 66 (4): 382-3; Guo Hongzhu, Yuan Jiurong, limonium sinenseKuntze The Chemical Constituents. herbal medicine, 1994, (8); 398-400)).This plant have enrich blood, hemostasis, antisepsis and anti-inflammation, the loose stasis of blood, menstruation regulating, beneficial spleen, multiple pharmacological effect such as be good for the stomach, be mainly used in treatment dysfunctional uterine hemorrhage disease clinically.Scholars mainly concentrate on antibiotic, antiviral, the aspect of tonifying the blood and arrest bleeding (Lin LC to its Pharmacological action study at present, Kuo YC, Chou CJ.Anti-herpes simplex virustype-1flavonoids and a new flavanone from the root of Limonium sinense.Planta Med.2000,66 (4): 333-336; Sweet dew, Zhao Yuying. Statice compounds research overview. northwest pharmaceutical journal .1997,12 (3) .:135-140).We in early stage discover that the limonium sinenseKuntze root extract has activity (Tang Xinhui, the Gao Jing significantly antitumor and damage of antagonism normal cell, Xu Li causes, Deng. limonium sinenseKuntze is used to prepare the purposes (ZL200610086169.9) of antitumor drug, national inventing patent, 2008; Xinhui Tang, Jing Gao, Jin Chen, et al.Expression of VDAC regulated by extractsof Limonium sinense Ktze root against CCl
4-induced liver damage.International Journal ofMolecular Sciences.2007,8; 204-213; Xinhui Tang, Jing Gao, Jin Chen, et al.Mitochondrial modulationis involved in the hepatoprotection of Limonium sinense extract against liver damage in mice.Journal of Ethnopharmacology.2008,120 (3); 427-431).
Polysaccharide is by the natural macromolecular material of ten to up to ten thousand monosaccharide groups with the glycosidic link be combined into, because its molecular formula is (CH
2O)
nSo, be called " carbohydrate " again.It belongs to the non-cytotoxicity material, great advantage as medicinal application is that toxic side effect is less, and wide material sources, therefore, active polysaccharide can be used as ideal and effectively biochemical drug and functional food (the Chen Huili chief editor. the structure of saccharide complex and function. press of Shanghai Medical Univ, 1997:336.).Polysaccharide has many effects, antitumor and enhance immunity function be one of them mainly act on (State of Zhao China, Li Zhixiao, Chen Zongdao. the structural analysis of Chinese yam polysaccharide RDPS-I and anti-tumor activity. Acta Pharmaceutica Sinica, 2003,38 (1): 37-41; Hu Guoqiang, Yang Baohua, Zhang Zhongquan. Chinese yam polysaccharide is to the influence of rat blood sugar and pancreas islet release. Shandong journal of traditional Chinese medicine, 2004,23 (4): 230-231).
Summary of the invention
The invention discloses a kind of preparation method of limonium sinenseKuntze polysaccharide, the present invention is optimized on the technology that conventional polysaccharide extracts, and extracts the extraction rate reached to 12.80% of the limonium sinenseKuntze polysaccharide that obtains.
Extracting method of the present invention comprises: with the full root drying of limonium sinenseKuntze, pulverize, with distilled water extraction 1～3 time, united extraction liquid, concentrate, ethanol sedimentation, taking precipitate lyophilize, that is, wherein extracting temperature is 90 ℃～100 ℃, water-bath is ultrasonic before extracting, and ultrasonic time is 40min～60min.
In the said extracted method solid-liquid ratio of limonium sinenseKuntze and distilled water select 1: 8～1: 15.The more preferably weightmeasurement ratio of limonium sinenseKuntze and distilled water is 1: 12.
Extract temperature in the said extracted method and be preferably 95 ℃.
The preferred 50min of ultrasonic time during extraction.
With the distilled water extraction number of times preferred 2 times.
In the said extracted method, precipitation alcoholic acid weight percent concentration preferred 95%.
The extraction rate reached to 12.80% of the limonium sinenseKuntze polysaccharide that the present invention makes (being called for short LSEP).Antioxidtive Activities in Vitro is better, and 80 μ g/ml LSEP remove DPPH and reach 97%, 600 μ g/ml LSEP and remove ABTS and reach 97%, 1000 μ g/mlLSEP and remove OH. and reach 70%.
The invention will be further elaborated below in conjunction with embodiment.
Description of drawings
Fig. 1 is the influence of extraction time to the limonium sinenseKuntze polysaccharide yield
Fig. 2 extracts the influence of temperature to the limonium sinenseKuntze polysaccharide yield
Fig. 3 is the influence of ultrasonic time to the limonium sinenseKuntze polysaccharide yield
Fig. 4 is the influence of extraction time to the limonium sinenseKuntze polysaccharide yield
Fig. 5 is the influence of solid-liquid ratio to the limonium sinenseKuntze polysaccharide yield
Fig. 6 is a ultrasonic time and the response surface figure that extracts temperature in the response surface
Fig. 7 is a ultrasonic time and the isogram that extracts temperature in the response surface
Fig. 8 is a solid-liquid ratio and the response surface figure that extracts temperature in the response surface
Fig. 9 is a solid-liquid ratio and the isogram that extracts temperature in the response surface
Figure 10 is the response surface figure of solid-liquid ratio and ultrasonic time in the response surface
Figure 11 is the isogram of solid-liquid ratio and ultrasonic time in the response surface
Embodiment
Embodiment 1
With the full root drying of limonium sinenseKuntze, pulverize, use distilled water extraction, united extraction liquid, concentrated, ethanol sedimentation, taking precipitate lyophilize promptly get the limonium sinenseKuntze polysaccharide.
The single-factor influence experiment of 1, extracting
The factor that influences polysaccharide extract rate is a lot, this experiment selected temperature, time, solid-liquid ratio, extraction time, its influence to polysaccharide extract rate of 5 Study on influencing factors of ultrasonic wave.
Choose test and extract 60 ℃ of temperature, 70 ℃, 80 ℃, 90 ℃ and 100 ℃ of five levels; Extraction time chooses 1,2, and 3,4 and five levels of 5h; Solid-liquid ratio is chosen 1: 8, and 1: 10,1: 12,1: 14,1: 16 five level; Extraction time chooses 1,2,3,4 four levels; Ultrasonic time is chosen 20min, 40min, 60min, 80min; Carry out single factor experiment respectively.
1.1 extraction time influence Fig. 1 for 100 ℃ of temperature, solid-liquid ratio 1: 12, extraction time 2h, ultrasonic 20min the time different extraction times to the influence of polysaccharide yield.
As shown in Figure 1, extraction time is in 3 times, and polysaccharide yield increases obviously, and 3 increases later on slowly.Therefore extraction time is advisable for 2～3 times.
1.2 differing temps is to the influence of polysaccharide yield when Temperature Influence Fig. 2 is solid-liquid ratio 1: 12, extraction time 2h, ultrasonic 20min, when extracting 2 times.
As shown in Figure 2, along with the rising of extracting temperature, polysaccharide yield constantly increases, and increases comparatively remarkable before 70 ℃, increase later on not too obvious, temperature 70,80 rate curve is comparatively mild, simultaneously as can be seen from the polysaccharide soln that extracts, along with the rising of temperature, the polysaccharide color burn.Can draw thus, high temperature may have certain influence with active to the structure of polysaccharide, surpass 100 ℃ of polysaccharide and decompose easily and produce monose and be dissolved in the dense ethanol and then influence the extraction yield of polysaccharide, so select 90 ℃～100 ℃ as extractions than optimal temperature.
1.3 the supersound extraction time influence Fig. 3 for 100 ℃ of temperature, solid-liquid ratio 1: 12, extraction time 2h, when extracting 2 times different ultrasonic times to the influence of polysaccharide yield.
Known that by Fig. 3 ultrasonic time is between 20～40min, polysaccharide yield is constant substantially, along with the increase of ultrasonic time, polysaccharide yield constantly increases, but after ultrasonic time is more than 60min, the yield of polysaccharide reduces on the contrary gradually, during therefore ultrasonic 60min, and the polysaccharide yield maximum.
1.4 extraction time influence Fig. 4 for 100 ℃ of temperature, solid-liquid ratio 1: 12, extract 2 times, during ultrasonic 20min different extraction times to the influence of polysaccharide yield.
Known that by Fig. 4 along with the increase of heat-up time, polysaccharide extract rate increases before 2h significantly, increase later on is comparatively mild, increases to the later polysaccharide extract rate of certain hour and almost remains unchanged.May promote the dissolving of polysaccharide to make extraction yield increase, but heat-up time, long extraction yield not have considerable change, considered economic benefit because heat-up time is long, extraction time selects 2～3h to be advisable.
1.5 the influence of the influence of liquid material ratio different feed liquid comparison polysaccharide yield when 100 ℃ of temperature, extraction time 2h, extraction 2 times, ultrasonic 20min.
As shown in Figure 5, owing to extract the increase of the water yield, the amount that the polysaccharide of extraction is dissolved in the water is just many more, and the polysaccharide amount of loss is just few more, and corresponding polysaccharide extract rate is just high, and therefore along with the increase gradually of amount of water, polysaccharide yield increases gradually; But after increasing to a certain degree, polysaccharide extract rate is almost constant, and the extraction yield that increases water yield polysaccharide again reduces on the contrary, so solid-liquid ratio selects be advisable at 1: 12.
To sum up experiment of single factor extracts 90 ℃～100 ℃ of temperature; Extraction time is chosen 2～3h; Solid-liquid ratio is chosen 1: 12; Extraction time is chosen 2～3 times; Ultrasonic time is chosen 40min～60min, is preferred extraction scope.
2 adopt the optimization of response surface analysis method to limonium sinenseKuntze polysaccharide water extraction process
(1) the response surface analysis level of factor chooses
Center combination experimental design principle according to Box-Benhnken, comprehensive single-factor influence experimental result, choose and extract temperature, ultrasonic time, solid-liquid ratio limonium sinenseKuntze polysaccharide water is put forward significant three factors of influence, adopt the response surface analysis method of three factors, three levels on the basis of single factor experiment, experimental factor and level design see Table 1.
Table 1 response surface analysis factor and level
(2) response surface analysis scheme and result
To do conversion as follows to extracting temperature Z1, ultrasonic time Z2 and solid-liquid ratio Z3: X1=(Z1-90)/10, X2=(Z2-40)/20, X3=(Z3-12)/2.With X1, X2, X3 is an independent variable(s), is response value (Y) with the polysaccharide extract rate, testing program and test-results see Table 2.
Table 2 response surface analysis scheme and experimental result
Test number X1 X2 X3 polysaccharide extract rate/%
1 -1 -1 0 7.728
2 -1 0 -1 6.082
3 -1 0 1 6.326
4 -1 1 0 6.926
5 0 -1 -1 10.976
6 0 -1 1 8.972
7 0 1 1 9.936
8 1 -1 0 9.552
9 1 0 -1 9.24
10 1 0 1 11.082
11 1 1 0 13.11
12 0 1 -1 9.852
13 0 0 0 12.96
14 0 0 0 12.88
15 0 0 0 12.94
15 test points are divided into factorial point and zero point, and 1～12nd, factorial test, 13～15th, center test.Wherein factorial point is that the independent variable(s) value is at X
1, X
2, X
3The three-dimensional vertices that is constituted; Be the central point in zone zero point, and zero point, test repeated 3 times, in order to estimate testing error.
Adopt Design-Expert 7.0.0Trial program that the gained data are carried out regression analysis, regression analysis the results are shown in Table 3, and respond face figure and isogram, sees Fig. 6-11 respectively.
Table 3 regression analysis result
Each factor solves regression equation and is behind regression fit:
Y＝12.96+1.99X
1+0.35X
2-1.75E3X
3+1.09X
1X
2+0.40X
1X
3+0.57X
2X
3-2.67X
1 2-0.96X
2 2-2.11X
3 2
As known from Table 3, when describing concerning between each factor and the response value with above-mentioned regression equation, the linear relationship between its dependent variable and all independent variable(s) is (R significantly
2=0.9624), the P=0.0046 of equation, highly significant, on another kind of meaning, this experimental technique is reliable.Can find out also that from the further check of the every variance of regression equation it is very little that item is intended in the mistake of equation, shows that this equation is good to the experimental fit situation, experimental error is little, and therefore available this regression equation replaces true the putting of experiment that experimental result is analyzed.The every The results of analysis of variance of regression equation shows that also the equation once influence of item, quadratic term all is significant, so influence of each concrete experiment factor pair response value is not simple linear relationship.
The influence of each factor to response value reflected in Fig. 6～11, exists the condition of extreme value should be at circle centre position as can be seen by isogram.Relatively three picture groups as can be known: extract temperature (X
1) the most remarkable to the influence of limonium sinenseKuntze polysaccharide lixiviate, it is steeper to show as curve; And ultrasonic time (X
2) and solid-liquid ratio (X
3) take second place, it is comparatively level and smooth to show as curve, and with the increase or the minimizing of its numerical value, response value changes less.
For the further value of conclusive evidence optimum point, regression equation is got the single order partial derivative equals zero and put in order:
1.99-2*2.67X
1+1.09X
2+0.40X
3＝0 (1)
0.35+1.09X
1-2*0.96X
2+0.57X
3＝0 (2)
0.00175+0.40X
1+0.57X
2-2*2.21X
3＝0 (3)
The solving equation group gets X
1=0.480613, X
2=0.488113, X
3=0.111071, get Z after the conversion
1=94.80613, Z
2=49.76226, Z
3=12.222142, promptly the limonium sinenseKuntze water top condition of carrying polysaccharide is for extracting 94.81 ℃ of temperature, ultrasonic time 49.76min, solid-liquid ratio 1: 12, and with this understanding, limonium sinenseKuntze polysaccharide extract rate theoretical value can reach 13.5%.
Reliability for checking R SA method, the water that adopts above-mentioned optimum extraction conditions to carry out polysaccharide is proposed test, consider the facility of actually operating simultaneously, limonium sinenseKuntze water is put forward the polysaccharide top condition to be modified to and to extract 95 ℃ of temperature, ultrasonic time 50min, solid-liquid ratio at 1: 12 o'clock, the actual extraction yield that records is 13.0%, compares relative error about 4% with the theoretical prediction value.Therefore, the extracting condition parameter that the optimization of employing RSA method obtains has practical value accurately and reliably.
Application responds surface analysis method is optimized the extraction process of limonium sinenseKuntze polysaccharide, thereby try to achieve the optimum process condition that limonium sinenseKuntze polysaccharide water carries is: extract 95 ℃ of temperature; Ultrasonic time 50min; Solid-liquid ratio 1: 12; When extracting 2 times, the extraction rate reached of limonium sinenseKuntze polysaccharide is to 12.80%.
The preparation of limonium sinenseKuntze polysaccharide
Dry limonium sinenseKuntze root is pulverized, and accurately takes by weighing 200g, adds distilled water 2400ml, and behind the ultrasonic 50min, temperature is controlled at 95 ℃, and refluxing extraction 2 hours is filtered; Filter residue is used 2400ml distilled water refluxing extraction 2 hours again; Merge twice filtrate, concentrating under reduced pressure, with 95% ethanol alcohol precipitation, wave alcohol, lyophilize, the brown dry powder 26.0g of polysaccharide.
Embodiment 3
The preparation of limonium sinenseKuntze polysaccharide:
Dry limonium sinenseKuntze root is pulverized, and accurately takes by weighing 200g, adds distilled water 2400ml, and behind the ultrasonic 40min, temperature is controlled at 90 ℃, and refluxing extraction 2 hours is filtered; Filter residue is used 2000ml distilled water refluxing extraction 2 hours again; Merge twice filtrate, concentrating under reduced pressure, with 95% ethanol alcohol precipitation, wave alcohol, lyophilize, the brown dry powder 25.76g of polysaccharide.
The preparation of limonium sinenseKuntze polysaccharide:
Dry limonium sinenseKuntze root is pulverized, and accurately takes by weighing 200g, adds distilled water 2800ml, and behind the ultrasonic 60min, temperature is controlled at 90 ℃, and refluxing extraction 2 hours is filtered; Filter residue is used 2800ml distilled water refluxing extraction 2 hours again; Merge twice filtrate, concentrating under reduced pressure, with 95% ethanol alcohol precipitation, wave alcohol, lyophilize, the brown dry powder 19.872g of polysaccharide.
Claims (7)
1. the extracting method of a limonium sinenseKuntze polysaccharide, comprise: with the full root drying of limonium sinenseKuntze, pulverize, with distilled water extraction 1～3 time, united extraction liquid, concentrate, ethanol sedimentation, taking precipitate lyophilize, promptly, it is characterized in that: extracting temperature is 90 ℃～100 ℃, and water-bath is ultrasonic before extracting, and ultrasonic time is 40min～60min.
2. the extracting method of claim 1, wherein the weightmeasurement ratio of limonium sinenseKuntze and distilled water is 1: 8～1: 15.
3. the extracting method of claim 2, wherein the weightmeasurement ratio of limonium sinenseKuntze and distilled water is 1: 12.
4. the extracting method of claim 1, wherein extracting temperature is 95 ℃.
5. the extracting method of claim 1, wherein ultrasonic time 50min.
6. the extracting method of claim 1 is wherein used distilled water extraction 2 times, each 2～3 hours extraction times.
7. the preparation method of claim 1, wherein the alcoholic acid weight percent concentration is 95%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040056351A (en) * | 2002-12-23 | 2004-06-30 | 김영재 | Concentrate concentrated the components contained in the pear scent and extracting method of the concentrate. |
| CN1602687A (en) * | 2004-08-19 | 2005-04-06 | 中国农业大学 | Limonium cut flower pretreatment solution and method of use thereof |
| CN1927237A (en) * | 2006-09-06 | 2007-03-14 | 盐城师范学院 | Use of Chinese sealavender for preparing antineoplastic drug |
| CN101392031A (en) * | 2008-11-10 | 2009-03-25 | 马宏达 | Extraction and separation method of inonotus obliquus polysaccharide |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040056351A (en) * | 2002-12-23 | 2004-06-30 | 김영재 | Concentrate concentrated the components contained in the pear scent and extracting method of the concentrate. |
| CN1602687A (en) * | 2004-08-19 | 2005-04-06 | 中国农业大学 | Limonium cut flower pretreatment solution and method of use thereof |
| CN1927237A (en) * | 2006-09-06 | 2007-03-14 | 盐城师范学院 | Use of Chinese sealavender for preparing antineoplastic drug |
| CN101392031A (en) * | 2008-11-10 | 2009-03-25 | 马宏达 | Extraction and separation method of inonotus obliquus polysaccharide |
Non-Patent Citations (1)
| Title |
|---|
| 《天津农学院学报》 20091231 甄润英、张欢、李晓雁、王惠 二色补血草多糖的提取及抗氧化功能研究 17-20 1-7 第16卷, 第4期 2 * |
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