CN105693877A - Preparation and detection method of medicine mulberry polysaccharide extract - Google Patents
Preparation and detection method of medicine mulberry polysaccharide extract Download PDFInfo
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- CN105693877A CN105693877A CN201610138434.7A CN201610138434A CN105693877A CN 105693877 A CN105693877 A CN 105693877A CN 201610138434 A CN201610138434 A CN 201610138434A CN 105693877 A CN105693877 A CN 105693877A
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- G01N27/447—Systems using electrophoresis
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Abstract
The invention discloses a preparation method of a medicine mulberry polysaccharide extract. The preparation method comprises steps as follows: (1) medicine mulberry powder and distilled water are mixed and subjected to ultrasonic extraction twice at 60 DEG C, extraction is performed for 30 min each time, the solid-to-liquid ratio is 1:10, mixtures are filtered, and filtrates are mixed and concentrated; (2) a concentrated liquid obtained through concentration in the step (1) and ethanol are mixed in the volume ratio being 1:4, and the mixture is left to stand for alcohol precipitation for 24 h; (3) precipitate obtained through alcohol precipitation in the step (2) is subjected to reduced-pressure drying, and the medicine mulberry polysaccharide extract is obtained. Compared with a water bath extraction method, the preparation method can obviously increase the yield of the medicine mulberry polysaccharide extract. The invention further provides a detection method of the medicine mulberry polysaccharide extract with a high-performance capillary electrophoresis method. The detection method has good repeatability, stability and precision and can be used for evaluation of medicine mulberry extraction quality, so that stable control on the extraction quality is realized.
Description
Technical field
The present invention relates to the preparation of a kind of medicine Mulberry polyoses extract and detection method thereof。
Background technology
The black Mulberry kind (MorusnigraLinn) of medicine Morus, for natural 22 times of body half wild Mulberry Germplasm Resources of cultivated form, only it is distributed in Aksu of Xinjiang and field and Kaxgar Prefecture, it is the medicinal fruit Mulberry germ plasm resource of Xinjiang uniqueness, medicine Fructus Mori is especially as the medical material among the people that the Uygur nationality is important, and the Uygur nationality is called " summer figure soil "。Energy invigorating brain and relieving mental uneasiness, strengthening the spleen stomach, replenishing blood and nourishing liver, be used for treating the diseases such as palpitation and insomnia, forgetful, Deficiency and coldness of spleen and stomach and icterohepatitis。
High performance capillary electrophoresis (HPCE) be the one that developed recently gets up have efficiently quick, highly sensitive, automatization is high, the advantage such as economic and environment-friendly, become a kind of separate analytical technique with fastest developing speed in biochemistry and analytical chemistry field, cause the extensive attention of pharmaceutical analysis circle。But there is also the shortcoming such as poor reproducibility, preparative capacibility difference。
So far, prior art is generally adopted water boiling and precipitation with ethanol method and extracts medicine Mulberry polysaccharide, but polysaccharide yield is not high。And lacking a kind of method that medicine Mulberry polyoses extract is evaluated so that the quality of extract is uneven, is unfavorable for industrialized production。
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of prior art, it is provided that the preparation method of a kind of medicine Mulberry polyoses extract, to improve the productivity of medicine Mulberry polyoses extract。
It is a further object of the present invention to provide the detection method of a kind of medicine Mulberry polyoses extract, be evaluated with the extraction quality to medicine Mulberry, it is achieved control to extract stablizing of quality。
In order to solve above-mentioned technical problem, the invention provides following technical scheme:
The preparation method of a kind of medicine Mulberry polyoses extract, comprises the steps:
(1) medicine Mulberry powder and distilled water are mixed, supersound extraction twice at 60 DEG C, extract 30 minutes, solid-liquid ratio 1:10(g/mL every time), filter, merging filtrate, concentration；
(2) concentrated solution that step (1) concentration obtains is mixed with ethanol 1:4 by volume, stand precipitate with ethanol 24 hours；
(3) the precipitation drying under reduced pressure obtained by step (2) precipitate with ethanol, namely obtains medicine Mulberry polyoses extract。
Further, during step (1) supersound extraction, ultrasonic frequency is 59KHz。
Further, the volume after the concentration of step (1) filtrate is 1mL:1g with the mass ratio of medicine Mulberry powder。
The detection method of a kind of medicine Mulberry polyoses extract, comprises the steps:
(1) medicine Mulberry polyoses extract carries out acid hydrolysis in trifluoroacetic acid aqueous solution, after acid hydrolysis, removes trifluoroacetic acid, and residue with water dissolves, and obtains test liquid；
(2) derivatization of monosaccharide mixed standard solution: add 1-phenyl-3-methyl-5-pyrazolones ketone in monosaccharide mixed standard solution, reacting by heating in the basic conditions, cooling, acid adding neutralizes, then extract with chloroform, taking upper liquid, described monosaccharide is glucose, mannose, galactose, rhamnose, galacturonic acid, xylose and/or arabinose；
(3) capillary electrophoresis apparatus detection in upper liquid step (2) obtained, it is thus achieved that the standard curve of concentration and peak area, deposition condition: buffer adopts concentration to be the borate buffer solution of 180mmol/L, pH=10.05, voltage 15kV detects wavelength 245nm；
(4) test liquid of step (1) first processes by the derivatization method of step (2), then by capillary electrophoresis apparatus detection on the deposition condition of step (3)；
(5) detect the standard curve of peak area and the step (3) obtained according to step (4), obtain the concentration of glucose in test liquid, mannose, galactose, rhamnose, galacturonic acid, xylose and/or arabinose。
Further, step (1) acid hydrolysis 4 hours at 105 DEG C, the concentration 2mol/L of trifluoroacetic acid aqueous solution。
Further, after step (1) acid hydrolysis, adding methanol to system, evaporation and concentration removes trifluoroacetic acid。
Further, step (2), under the alkali condition of pH=10-12, reacts 30min in 70 DEG C。
During derivatization, for monosaccharide, the consumption of 1-phenyl-3-methyl-5-pyrazolones ketone keeps excessive。
Compared with extracting with water-bath, the present invention adopts ultrasonic assistant to extract the productivity that can significantly improve medicine Mulberry polyoses extract。And detection method provided by the invention has good repeatability, stability and precision, thus can be used for evaluating medicine Mulberry to extract quality, to realize the stability contorting of extraction quality。
Accompanying drawing explanation
Accompanying drawing is for providing a further understanding of the present invention, and constitutes a part for description, is used for together with embodiments of the present invention explaining the present invention, is not intended that limitation of the present invention。In the accompanying drawings:
Fig. 1 is the capillary electrophoresis spectrogram of monosaccharide hybrid standard product PMP derivant；
Fig. 2 is the capillary electrophoresis spectrogram of PMP derivant after the hydrolysis of medicine Mulberry polyoses extract。
Detailed description of the invention
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is merely to illustrate and explains the present invention, is not intended to limit the present invention。
1.1 materials and reagent
Medicine Mulberry picks up from-----Kashgar 20120810-1 in the period of maturation, pharmaceutical college of Xinjiang Medicine University professor Pa Lida be accredited as medicine Sang Heisang kind。
Monosaccharide standard substance: glucose (D-Glucoseanhydrous, 110833-200904), mannose (Mannose, 140651-200602), galactose (Galactose100226-201105), rhamnose (Rhamnose, 111683-200401), galacturonic acid (GalUA), xylose (D-xylose, 111508-200404), arabinose (Arabinose, 1506-200001) (above reagent equal Chinese food medicine identification research institute)。
Reagent: methanol, dehydrated alcohol, chloroform, trifluoroacetic acid (TFA), (above reagent Tianjin Fu Yu Fine Chemical Co., Ltd, analytical pure)；HCl, NaOH(are all from Luoyang City's chemical reagent factory, analytical pure)；Ultra-pure water (Ai Ke)。
Derivatization reagent: 1-phenyl-3-methyl-5-pyrazolones ketone (PMP, analytical pure, Shanghai reagent two factory)。
1.2 instruments
Capillary electrophoresis apparatus P/ACE(Benkman company) PDA detector；32KaratSofware；Capillary column (sharp Feng chromatograph Devices of Yongnian County, non-coating, d=75mm)；Analytical balance (Beijing Sai Duolisi balance company limited, Sartorius, BS110S, d=0.1mg)；PH meter (Shanghai thunder magnetic phsj-3F, Shanghai Yi electricity science limited company)；Vacuum drying oven；Ultrasound Instrument (KQ-500PE type, Kunshan Ultrasonic Instruments Co., Ltd.)；Water-bath (DZKW-S-4 Beijing is bright Medical Instruments company limited forever)。
2 methods and result
The preparation precision of 2.1 medicine Mulberry polyoses extracts weighs 10g medicine Mulberry powder to conical flask, and precision measures 100mL ultra-pure water and adds conical flask, supersound extraction, filtering, residue is supersound extraction again, and the temperature of each supersound extraction is 60 DEG C, ultrasonic frequency 59KHz, extraction time is 30min。Merge the filtrate of twice supersound extraction, being transferred in beaker by filtrate, be concentrated into about surplus 10mL with Rotary Evaporators subsequently, concentrated solution produces to beaker, then by ethanol: the volume ratio of concentrated solution=4:1 adds ethanol and carries out precipitate with ethanol, room temperature stands 24h, abandoning supernatant, and precipitation is transferred to evaporating dish, put into decompression oven drying 12h, taking out drying solid, be medicine Mulberry polyoses extract, the productivity of medicine Mulberry polysaccharide is 12.20%。
Control experiment: precision weighs 10g medicine Mulberry powder to conical flask, precision measures 100mL ultra-pure water and adds conical flask, and water-bath is extracted, and filters, and residue water-bath again is extracted, and the temperature every time extracted is 60 DEG C, and ultrasonic frequency 59KHz, extraction time is 2 hours。Merge the filtrate that twice water-bath is extracted, filtrate is transferred in beaker, it is concentrated into about surplus 10mL subsequently with Rotary Evaporators, concentrated solution produces to beaker, then by ethanol: the volume ratio of concentrated solution=4:1 adds ethanol and carries out precipitate with ethanol, and room temperature stands 24h, abandoning supernatant, precipitation being transferred to evaporating dish, puts into decompression oven drying 12h, the productivity of medicine Mulberry polysaccharide is 11.52%。Productivity=polysaccharide/medicine Mulberry powder, medicine Mulberry polysaccharide adopts phend-sulphuric acid to measure。
The detection of 2.2 medicine Mulberry polyoses extracts
2.2.1 the hydrolysis of medicine Mulberry polyoses extract accurately weighs above-mentioned medicine Mulberry polyoses extract 10mg and is placed in peace and cuts open bottle, after adding 2mL2mol/LTFA (trifluoroacetic acid) aqueous solution, it is placed in 105 DEG C of baking ovens, acid hydrolysis 4h, then add methanol to this test solution and rotate evaporation and concentration, concentrate three times (too dry first twice, third time concentration is dry, adds 3mL methanol every time), use ultra-pure water dissolved residue again, it is transferred to 5mL volumetric flask, constant volume, obtains test liquid。
2.2.2 derivatization treatment
2.2.2.1 the derivatization of monosaccharide mixed standard solution
Compound concentration is the standard solution of 20mmol/L glucose, mannose, galactose, rhamnose, galacturonic acid, xylose and arabinose respectively。
Respectively precision draws above-mentioned each monosaccharide standard solution in 10mL volumetric flask, uses ultra-pure water constant volume, mixing, obtain a series of (concentration 0.03125,0.0625,0.125,0.25,0.5,0.75,1,2mmol/L) monosaccharide mixed standard solution。
Taking monosaccharide mixed standard solution 500 μ L in tool plug test tube, add 500 μ L0.3mol/LPMP methanol solutions and 500 μ L0.3mmol/LNaOH solution, vortex 30s, be subsequently placed in 70 DEG C of water-bath 30min, be cooled to room temperature, dropping 0.3mmol/LHCl solution is neutralized。Adding 2mL chloroform again, spin upside down 10 times, discard subnatant, repeat 2 times, draw supernatant liquid, cross 0.45 μ L filter membrane, filtrate is to sample injection bottle。
2.2.2.2 the derivatization of sample
The accurate test liquid 500 μ L drawn under 2.2.1 item, performs the derivatization test liquid according to the method under 2.2.2.1 item。
2.2.3 detect
Sample derivatization treatment under 2.2.2 item obtained is gone up capillary electrophoresis apparatus respectively and is detected, deposition condition: buffer adopts the borate buffer solution of concentration 180mmol/LpH=10.05, voltage 15kV, detects wavelength 245nm, sample introduction 10s under air pressure sample introduction 0.5psi, column temperature 25 DEG C。
Before capillary electrophoresis apparatus uses every time, respectively rinse 3min with water, 0.1mol/LNaOH, water, 0.1mol/LHCl, water, buffer successively, then balance 5min with buffer。
The capillary electrophoresis spectrogram of monosaccharide hybrid standard product PMP derivant is as shown in Figure 1, after the hydrolysis of medicine Mulberry polyoses extract, the capillary electrophoresis spectrogram of PMP derivant is as shown in Figure 2, wherein each peak is respectively as follows: 1-xylose, 2-arabinose, 3-glucose, 4-rhamnose, 5-mannose, 6-galactose, 7-galacturonic acid。By Fig. 1-2 it can be seen that the peak that PMP produces can separate well with each monosaccharide derivatives, do not affect the mensuration of sample。
Test result indicate that, separation is had obvious impact by the acidity of buffer and concentration。The separating degree of 7 kinds of monosaccharide standard substance PMP derivants increases with borate buffer pH value and improves, and meanwhile, increases borate concentration in buffer, and separating degree improves, but the appearance time of monosaccharide also extends to some extent, and electric current increases more apparent, affects repeatability。
2.2.4 standard curve
With the concentration X of a series of monosaccharide mixed standard solutions for abscissa, peak area Y is that vertical coordinate carries out linear regression, obtains regression equation。Result is in Table 1
The regression equation of each monosaccharide of table 1
2.2.5 sample size measures
By the collection of illustrative plates of medicine Mulberry polyoses extract test liquid and monosaccharide hybrid standard spectral contrast, by corresponding peak area and standard curve, the concentration of glucose in test liquid, mannose, galactose, rhamnose, galacturonic acid, xylose and arabinose can be obtained, correction factor is adopted to calculate the ratio of each monosaccharide in test liquid, to evaluate medicine Mulberry extraction quality, it is achieved the stability contorting of quality。After the hydrolysis of medicine Mulberry polyoses extract sample, the percent of monosaccharide component, migration time and peak area is as follows:
2.3 repeated experiments
Taking with a collection of medicine Mulberry sample, process by the method under 2.2, sample introduction 6 times, in mensuration medicine Mulberry polysaccharide, the RSD of each contents of monosaccharides is 1%～6%, it was shown that this method is reproducible。Result is in Table 2
Table 2 replica test result
2.4 stability tests
Sample 0,2,4,6,8,12,24,48h respectively sample introduction measure as a result, each monosaccharide chromatographic peak area is without significant change in 48h, RSD respectively 3.76%, 1.20%, 1.24%, 5.34%, 3.07%, 2.83%, 6.62%, result shows that sample is good at 48h internal stability。
2.5 Precision Experiments
Take same monosaccharide mixed standard solution, continuous sample introduction 6 times, measure peak area。Precision Experiment meets the requirements。Result is in Table 3
Table 3 Precision test result
2.6 response rate experiments
Accurate monosaccharide hybrid standard liquid 0.4mL, 0.5mL, 0.6mL drawing 2mmol/L, obtains the reference substance test solution of basic, normal, high three concentration。By legal system available test sample solution below 2.2.1 item。Draw test solution and each 250 μ l of high, normal, basic reference substance test solution with liquid-transfering gun, each three parts, perform the derivatization rear sample introduction by method under 2.2.2 item and measure, calculate average recovery。Result is in Table 4
Table 4 determination of recovery rates result (n=6)
Last it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, although the present invention being described in detail with reference to previous embodiment, for a person skilled in the art, technical scheme described in foregoing embodiments still can be modified by it, or wherein portion of techniques feature carries out equivalent replacement。All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention。
Claims (8)
1. a preparation method for medicine Mulberry polyoses extract, comprises the steps:
(1) medicine Mulberry powder and distilled water are mixed, supersound extraction twice at 60 DEG C, extract 30 minutes, solid-liquid ratio 1:10 every time, filter, merging filtrate, concentration；
(2) concentrated solution that step (1) concentration obtains is mixed with ethanol 1:4 by volume, stand precipitate with ethanol 24 hours；
(3) the precipitation drying under reduced pressure obtained by step (2) precipitate with ethanol, namely obtains medicine Mulberry polyoses extract。
2. the preparation method of medicine Mulberry polyoses extract according to claim 1, it is characterised in that during step (1) supersound extraction, ultrasonic frequency is 59KHz。
3. the preparation method of medicine Mulberry polyoses extract according to claim 1, it is characterised in that the mass ratio of the volume after the concentration of step (1) filtrate and medicine Mulberry powder is 1mL:1g。
4. a detection method for medicine Mulberry polyoses extract, comprises the steps:
(1) medicine Mulberry polyoses extract carries out acid hydrolysis in trifluoroacetic acid aqueous solution, after acid hydrolysis, removes trifluoroacetic acid, and residue with water dissolves, and obtains test liquid；
(2) derivatization of monosaccharide mixed standard solution: add 1-phenyl-3-methyl-5-pyrazolones ketone in monosaccharide mixed standard solution, reacting by heating in the basic conditions, cooling, acid adding neutralizes, then extract with chloroform, taking upper liquid, described monosaccharide is glucose, mannose, galactose, rhamnose, galacturonic acid, xylose and/or arabinose；
(3) capillary electrophoresis apparatus detection in upper liquid step (2) obtained, it is thus achieved that the standard curve of concentration and peak area, deposition condition: buffer adopts concentration to be the borate buffer solution of 180mmol/L, pH=10.05, voltage 15kV detects wavelength 245nm；
(4) test liquid of step (1) first processes by the derivatization method of step (2), then by capillary electrophoresis apparatus detection on the deposition condition of step (3)；
(5) detect the standard curve of peak area and the step (3) obtained according to step (4), obtain the concentration of glucose in test liquid, mannose, galactose, rhamnose, galacturonic acid, xylose and/or arabinose。
5. the detection method of medicine Mulberry polyoses extract according to claim 4, it is characterised in that step (1) acid hydrolysis 4 hours at 105 DEG C, the concentration 2mol/L of trifluoroacetic acid aqueous solution。
6. the detection method of medicine Mulberry polyoses extract according to claim 4, it is characterised in that after step (1) acid hydrolysis, adds methanol to system, and evaporation and concentration removes trifluoroacetic acid。
7. the detection method of medicine Mulberry polyoses extract according to claim 4, it is characterised in that step (2), under the alkali condition of pH=10-12, reacts 30min in 70 DEG C。
8. the detection method of medicine Mulberry polyoses extract according to claim 4, it is characterised in that during derivatization, for monosaccharide, the consumption of 1-phenyl-3-methyl-5-pyrazolones ketone keeps excessive。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107966502A (en) * | 2017-11-01 | 2018-04-27 | 广西壮族自治区食品药品检验所 | The method for measuring Radix Salviae Miltiorrhizae polysaccharide hydrolysate-galacturonic acid |
-
2016
- 2016-03-11 CN CN201610138434.7A patent/CN105693877A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107966502A (en) * | 2017-11-01 | 2018-04-27 | 广西壮族自治区食品药品检验所 | The method for measuring Radix Salviae Miltiorrhizae polysaccharide hydrolysate-galacturonic acid |
| CN107966502B (en) * | 2017-11-01 | 2021-01-01 | 广西壮族自治区食品药品检验所 | Method for determining polysaccharide hydrolysate-galacturonic acid in salvia miltiorrhiza bunge |
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