CN111454321A - Method for separating and preparing high-purity saponin compound from paris polyphylla stems and leaves - Google Patents
Method for separating and preparing high-purity saponin compound from paris polyphylla stems and leaves Download PDFInfo
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Abstract
The invention discloses a method for separating and preparing high-purity saponin compounds from paris polyphylla stems and leaves, which comprises a paris polyphylla stem and leaf extraction step, a macroporous resin column passing step, an extract preparation step and a monomer compound separation preparation step. According to the method for separating and preparing the high-purity saponin compound from the paris polyphylla stems and leaves, the paris polyphylla saponin II and the dioscin are prepared from the paris polyphylla stems and leaves by adopting macroporous adsorption resin combined preparation liquid chromatography, so that the medicinal value of paris polyphylla can be fully utilized, waste is turned into wealth, meanwhile, the preparation chromatography is used as an effective means for separating and purifying natural products, and the method has the advantages of simplicity and convenience in operation, high product purity, high separation speed and the like.
Description
Technical Field
The invention relates to a method for separating and preparing high-purity saponin compounds from stems and leaves of rhizoma paridis.
Background
The Paris polyphylla is dried rhizome of Paris polyphylla Smith var.yunnanensis (Franch.) hand-Mazz or Paris polyphylla Smith var.chinesis (Franch.) Hara of the family Liliaceae, has the effects of clearing heat and removing toxicity, relieving swelling and dissipating blood stasis, cooling liver and arresting convulsion, is mainly used for treating symptoms such as sore throat, snake and insect bite, traumatic injury and the like, and is applied to more than 40 Chinese patent medicines such as Qushengde snake tablets, Gongxuening, Yunnan white drug and the like.
The paris polyphylla is used as a perennial herb, the living environment is harsh, wild resources are in short supply, underground rhizomes can be used as the medicine only after 3-5 years, and overground parts are abandoned, so that the resource waste is caused. Along with the increasing of the demand of the market for the paris polyphylla in recent years and the shortage of paris polyphylla market resources, the shortage of paris polyphylla resources can be relieved by developing overground parts of the paris polyphylla, the cost is saved, and waste materials are changed into things of value, so that the applicant carries out a series of researches on stems and leaves of the paris polyphylla, and finds that the stems and leaves of the paris polyphylla mainly contain saponins and flavonoid chemical components [ Wangfei, the extraction and purification process of total flavonoids in the stems and leaves of the paris polyphylla and the research on the antioxidant activity, Anhui agricultural science, 2019, 47(9): 164-; dioscin has effects of reducing blood lipid, resisting inflammation, resisting virus, resisting fungus, resisting allergy and tumor, and can be used for treating liver, kidney, brain, stomach, intestine injury and metabolic diseases [ such as radix Seu caulis Gmeliae, flos Tamarindi Indicae, Zhangmegayun, HUYANGYANG, LIHENGZHANG, medicinal value and chemical substance basis of Paris, Chinese traditional medicine journal 2015, 40(5):833 + 839; the modern pharmacological research progress of dioscin from Chenyaqin, Cao cham et al, the modern journal of Chinese and Western medicine combination, 2019, 23: 2613-.
Although the two saponin compounds can be separated by adopting the traditional column chromatography, the efficiency is low, the time is consumed, and the solvent consumption is large; the thin layer chromatography is simple and convenient to prepare, but the sample treatment amount has certain limitation. The preparative chromatography technique is an effective technique for separating and purifying natural products and chemical synthetic products due to the characteristics of high column efficiency, high speed and the like [ Jiadan, Chen Miao, Jade, Zhuzhen, Chaaifeng, Zhang.
Aiming at the situation that the stems and leaves of the paris polyphylla are mostly discarded, the resources are recycled in an effort, the medicinal value of the paris polyphylla is fully excavated, and the separation based on the traditional column chromatography is troublesome and labor-consuming and pollutes the environment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for separating and preparing high-purity saponin compounds from paris polyphylla stems and leaves.
The technical scheme for realizing the purpose is as follows: a method for separating and preparing high-purity saponin compounds from paris polyphylla stems and leaves comprises the following steps:
s1, extracting stems and leaves of rhizoma paridis: refluxing and extracting the stems and leaves of the paris polyphylla for 1-3 times by using an ethanol water solution with the volume concentration of 50-80%, and recovering ethanol under reduced pressure to obtain an extracting solution;
s2, macroporous resin column passing step: passing the extracting solution through macroporous adsorption resin, sequentially removing impurities by using water and an ethanol aqueous solution with the volume concentration of 20-40%, then carrying out enrichment elution by using the ethanol aqueous solution with the volume concentration of 50-90%, collecting ethanol aqueous solution eluent with the volume concentration of 50-90%, concentrating and drying to obtain a crude extract;
s3, the preparation method of the extract comprises the following steps: ultrasonically dissolving the crude extract by using acetonitrile aqueous solution with the volume concentration of 20-50%, centrifuging, and taking precipitate to obtain a paris polyphylla stem and leaf extract;
s4, a monomer compound separation preparation step, namely, separating and purifying the obtained paris polyphylla stem and leaf extract by adopting a preparation liquid chromatography, firstly preparing a mobile phase required by the preparation chromatography, then dissolving the paris polyphylla stem and leaf extract, then feeding the dissolved extract into a sample injection valve, respectively receiving a target flow fraction I and a target flow fraction II according to a detection map, and respectively carrying out L C-MS structure identification on the target flow fraction I and the target flow fraction II to determine that the target flow fraction I is paris polyphylla saponin II and the target flow fraction II is dioscin.
In the above method for separating and preparing the high-purity saponin compound from the stems and leaves of the paris polyphylla, in step S1, the stems and leaves of the paris polyphylla are heated and refluxed and extracted by using ethanol water solution with the volume concentration of 70%.
The method for separating and preparing the high-purity saponin compound from the paris polyphylla stems and leaves comprises the step S2 of sequentially removing impurities by using water and an ethanol water solution with the volume concentration of 30-40% through the macroporous adsorption resin with the model of AB-8, DM-130 or HPD-600, then eluting by using the ethanol water solution with the volume concentration of 70-90%, wherein the elution volume of water for removing impurities is 5-15 BV, the elution volume of an ethanol water solution for removing impurities is 10-20 BV, the elution volume of the ethanol water solution for eluting a target component is 10-20 BV, collecting the ethanol water solution eluent with the volume concentration of 70-90%, concentrating and drying to obtain the paris polyphylla stem and leaf crude extract.
In the step S3, acetonitrile aqueous solution with the volume concentration of 20-40% is used for ultrasonically dissolving the crude extract of the stems and leaves of the paris polyphylla, then the crude extract is centrifuged at the rotating speed of 5000-15000 r/min, and the precipitate is taken to obtain the extract of the stems and leaves of the paris polyphylla.
In the above method for separating and preparing high-purity saponin compounds from paris polyphylla stems and leaves, in step S4, the parameters of the preparation liquid chromatography are as follows:
chromatographic column Waters X Bridge prep C18OBD column (19 × 150mm, 5 μm);
mobile phase: the phase A is acetonitrile, the phase B is water, 0-24 min and 30-65% of acetonitrile; 24-27 min, 65% -95% acetonitrile; 27-35 min, 95% acetonitrile;
the flow rate is 15m L/min;
detection wavelength: and 203nm, and respectively receiving the target fraction I and the target fraction II according to the detection map.
In the method for separating and preparing the high-purity saponin compound from the paris polyphylla stems and leaves, the purities of the paris polyphylla saponin II and the dioscin are respectively more than 95 percent.
The method for separating and preparing the high-purity saponin compound from the paris polyphylla stems and leaves aims at the defects that the paris polyphylla stems and leaves are wasted, and the separation is troublesome and labor-consuming and pollutes the environment based on the traditional column chromatography, adopts the macroporous adsorption resin combined preparation liquid chromatography to prepare the paris polyphylla saponin II and the dioscin from the paris polyphylla stems and leaves, can fully utilize the medicinal value of the paris polyphylla stems and leaves and change waste into valuable, simultaneously adopts the preparation chromatography as an effective means for separating and purifying natural products, has the advantages of simple and convenient operation, high product purity, high separation speed and the like, and is easy to popularize and.
Drawings
FIG. 1 is a flow chart of the method for separating and preparing high-purity saponin compounds from the stems and leaves of Paris polyphylla according to the present invention;
FIG. 2A is a HP L C profile of the extract obtained in step S1;
FIG. 2B is a HP L C profile of the crude extract obtained in step S2;
FIG. 3A is a liquid chromatogram of rhizoma paridis extract;
FIG. 3B is a diagram of HP L C of target fraction I obtained by preparative chromatography;
FIG. 3C is a diagram of HP L C of target fraction II from preparative chromatography
FIG. 4 is HP L C of rhizoma paridis saponin II and dioscin standard product;
FIG. 5A is a mass spectrum of a target fraction I obtained by preparative liquid chromatography;
FIG. 5B is a mass spectrum of the target fraction II obtained by preparative liquid chromatography.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following detailed description is given with reference to the accompanying drawings:
example 1:
referring to fig. 1, a method for separating and preparing high-purity saponins compound from rhizoma paridis stem and leaf includes the following steps:
s1, extracting stems and leaves of rhizoma paridis, namely weighing about 100g of stems and leaves of rhizoma paridis, heating and refluxing the weighed stems and leaves of rhizoma paridis with 8 times of 70% ethanol aqueous solution for 2 times, wherein the extraction temperature is 80 ℃, filtering and combining the filtrates, and concentrating the filtrate at 60 ℃ under reduced pressure until no alcohol smell exists to obtain a concentrated extract, wherein the HP L C of the extract is shown in figure 2A;
s2, a step of passing through a macroporous resin column, which is to add a proper amount of water into the concentrated extracting solution, add the extracting solution into a chromatographic column filled with 300g of the processed HPD-600 type macroporous adsorption resin, stand and adsorb for 4 hours after the sample is loaded, then remove impurities by using 1500ml of water and 1500ml of ethanol water solution with the volume concentration of 30 percent in sequence, elute by using 2250ml of ethanol water solution with the volume concentration of 80 percent, collect the eluent of the ethanol water solution with the volume concentration of 80 percent, concentrate under reduced pressure to obtain 7.93g of powdery crude extract with the yield of 7.93 percent, and obtain an HP L C diagram of the crude extract as shown in figure 2B;
s3, the preparation method of the extract comprises the following steps: taking a proper amount of the crude extract, preparing a sample solution with the concentration of 10.13mg/ml by using an acetonitrile aqueous solution with the volume concentration of 30%, carrying out ultrasonic dissolution for 15min, centrifuging at 10000r/min for 5min, and then precipitating a part in the sample solution to obtain a paris polyphylla stem and leaf extract;
s4, a monomer compound separation preparation step: separating and purifying the extract by preparative liquid chromatography under the following conditions:
chromatographic column Waters X Bridge prep C18OBD column (19 × 150mm, 5 μm);
mobile phase: the phase A is acetonitrile, the phase B is water, 0-24 min and 30-65% of acetonitrile; 24-27 min, 65% -95% acetonitrile; 27-35 min, 95% acetonitrile;
the flow rate is 15m L/min;
detection wavelength: 203 nm;
receiving a target fraction I and a target fraction II according to a detection map (see figure 3A), and determining that the target fraction I is the rhizoma paridis saponin II and the target fraction II is the dioscin by respectively carrying out L C-MS structural identification on the target fraction I and the target fraction II.
And (3) detecting the purities of the target flow I and the target flow II:
purity detection is carried out by adopting a peak area normalization method, and the HP L C analysis conditions of purity detection comprise chromatographic column Agilent Zorbax SB-Aq (4.6 × 250mm,5 mu m), mobile phase acetonitrile-water 0-40 min, 30-65% acetonitrile, flow rate 0.8m L/min, sample introduction amount 20 mu L, detection wavelength 203nm and column temperature 25 ℃.
FIGS. 3B and 3C are HP L C of target fraction I and target fraction II obtained by preparative liquid chromatography, and FIG. 4 is HP L C of two saponin monomers.
By comparison with fig. 4, it can be seen from fig. 3B and 3C that the retention time of the chromatographic peaks of the target fraction I and the target fraction II are consistent with that of the standard of fig. 4. The purity of the target fraction I is 95.34 percent; the purity of the target fraction II was 96.17%.
L C-MS structural identification of the target fraction:
referring to FIG. 5A and FIG. 5B, mass spectrometry of target fraction I and target fraction II, respectively, is performed, wherein the mass spectrometry comprises Agilent 6545Q-TOF L C-MS, chromatography column Agilent Zorbax SB-Aq (3.0 × 100mm,3.5 μm), mobile phase comprises acetonitrile-water 0-10 min, 30-70% acetonitrile, 10-12 min, 70-100% acetonitrile, flow rate 0.4m L/min, sample injection amount 3 μ L, detection wavelength 203nm, and column temperature 35 ℃.
Mass spectrum conditions of electrospray ionization source (ESI), positive ion time of flight (TOF) scanning mode, and flow rate of 8L & min-1At the temperature of 325 ℃; a fragment voltage of 135V; m/z 121.0508 and m/z 922.0098 are used as reference ions; electrospray voltage 35 psig; the collision energy is 25-30 eV.
Target fraction I, (M + Na)+1037.5288, consistent with the chromatographic retention time of the standard paris saponin II.
Target fraction II, (M + H)+,869.4884，(M+Na)+891.4702, consistent with the chromatographic retention time of the standard dioscin.
According to the structure identification result, the target fraction I is identified as the rhizoma paridis saponin II, and the target fraction II is identified as the dioscin.
Example 2:
referring to fig. 1, a method for separating and preparing high-purity saponins compound from rhizoma paridis stem and leaf includes the following steps:
s1, extracting stems and leaves of rhizoma paridis: weighing about 200g of rhizoma paridis stem and leaf, heating and reflux-extracting with 8 times of 80% ethanol at 90 deg.C for 2 times, each time for 2 hr, filtering, mixing filtrates, and concentrating under reduced pressure at 60 deg.C until no alcohol smell exists to obtain concentrated extractive solution;
s2, macroporous resin column passing step: adding a proper amount of water into the concentrated extracting solution, adding a chromatographic column filled with 500g of treated DM-130 type macroporous adsorption resin, standing and adsorbing for 4 hours after the sample loading is finished, then sequentially removing impurities by using 3000ml of water and 2000ml of ethanol water solution with the volume concentration of 40%, then eluting by using 4000ml of ethanol water solution with the volume concentration of 80%, collecting ethanol water solution eluent with the volume concentration of 80%, and concentrating under reduced pressure to obtain 15.89g of powdery crude extract with the yield of 7.95%;
s3, the preparation method of the extract comprises the following steps: taking a proper amount of the crude extract, preparing a sample solution with the concentration of 10.56mg/ml by using an acetonitrile aqueous solution with the volume concentration of 40%, carrying out ultrasonic dissolution for 10min, centrifuging at 10000r/min for 10min, and precipitating a part in the sample solution to obtain a paris polyphylla stem and leaf extract;
s4, the steps of separating and preparing the monomeric compound, the method and the steps of separating and purifying the monomeric compound, detecting the purity and identifying the L C-MS structure are the same as the example 1.
Example 3:
referring to fig. 1, a method for separating and preparing high-purity saponins compound from rhizoma paridis stem and leaf includes the following steps:
s1, extracting stems and leaves of rhizoma paridis: weighing about 200g of rhizoma paridis stem and leaf, heating and reflux-extracting with 10 times of 60% ethanol at 90 deg.C for 3 times, each for 2 hr, filtering, mixing filtrates, and concentrating under reduced pressure at 60 deg.C until no alcohol smell exists to obtain concentrated extractive solution;
s2, macroporous resin column passing step: adding a proper amount of water into the concentrated extracting solution, adding a chromatographic column filled with 500g of treated AB-8 type macroporous adsorption resin, standing and adsorbing for 4 hours after the sample loading is finished, then sequentially removing impurities by using 2400ml of water and 2400ml of ethanol water solution with the volume concentration of 35%, then eluting by using 3000ml of ethanol water solution with the volume concentration of 90%, collecting ethanol water solution eluent with the volume concentration of 90%, and concentrating under reduced pressure to obtain 16.38g of powdery crude extract with the yield of 8.19%;
s3, the preparation method of the extract comprises the following steps: taking a proper amount of the crude extract, preparing a sample solution with the concentration of 10.81mg/ml by using acetonitrile water solution with the volume concentration of 25%, carrying out ultrasonic dissolution for 15min, centrifuging at 15000r/min for 5min, and precipitating a part in the sample solution to obtain a paris polyphylla stem and leaf extract;
s4, the steps of separating and preparing the monomeric compound, the method and the steps of separating and purifying the monomeric compound, detecting the purity and identifying the L C-MS structure are the same as the example 1.
In conclusion, the method for separating and preparing the high-purity saponin compound from the stems and leaves of the paris polyphylla fully excavates medicinal resources of the paris polyphylla, expands the medicinal range of the paris polyphylla, changes waste into valuable, and can obtain the paris polyphylla saponin monomer after the stems and leaves of the paris polyphylla are extracted and purified by macroporous adsorption resin combined preparation liquid chromatography: rhizoma paridis saponin II and dioscin, which have proved to have strong biological activity. The method adopts macroporous adsorption resin combined preparation liquid chromatography to separate and purify the extract of the stems and leaves of the paris polyphylla, is simple, convenient and quick, overcomes the defects of long separation period, complex operation and the like of the traditional method, has the advantages of high efficiency, convenience and high product purity, and is easy to popularize and use.
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as a limitation of the present invention, and that changes and modifications to the above described embodiments are within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (6)
1. A method for separating and preparing high-purity saponin compounds from paris polyphylla stems and leaves is characterized by comprising the following steps:
s1, extracting stems and leaves of rhizoma paridis: refluxing and extracting the stems and leaves of the paris polyphylla for 1-3 times by using an ethanol water solution with the volume concentration of 50-80%, and recovering ethanol under reduced pressure to obtain an extracting solution;
s2, macroporous resin column passing step: passing the extracting solution through macroporous adsorption resin, sequentially removing impurities by using water and an ethanol aqueous solution with the volume concentration of 20-40%, then carrying out enrichment elution by using the ethanol aqueous solution with the volume concentration of 50-90%, collecting ethanol aqueous solution eluent with the volume concentration of 50-90%, concentrating and drying to obtain a crude extract;
s3, the preparation method of the extract comprises the following steps: ultrasonically dissolving the crude extract by using acetonitrile aqueous solution with the volume concentration of 20-50%, centrifuging, and taking precipitate to obtain a paris polyphylla stem and leaf extract;
s4, a monomer compound separation preparation step, namely, separating and purifying the obtained paris polyphylla stem and leaf extract by adopting a preparation liquid chromatography, firstly preparing a mobile phase required by the preparation chromatography, then dissolving the paris polyphylla stem and leaf extract, then feeding the dissolved extract into a sample injection valve, respectively receiving a target flow fraction I and a target flow fraction II according to a detection map, and respectively carrying out L C-MS structure identification on the target flow fraction I and the target flow fraction II to determine that the target flow fraction I is paris polyphylla saponin II and the target flow fraction II is dioscin.
2. The method for separating and preparing the high-purity saponin compound from the paris polyphylla stems and leaves as claimed in claim 1, wherein in step S1, the paris polyphylla stems and leaves are heated and refluxed and extracted by using an ethanol water solution with the volume concentration of 70%.
3. The method for separating and preparing the high-purity saponin compound from the stem and leaf of the paris polyphylla as claimed in claim 1, wherein in step S2, the model of the macroporous adsorption resin is AB-8, DM-130 or HPD-600, water and ethanol water solution with the volume concentration of 30% -40% are sequentially used for removing impurities, then the ethanol water solution with the volume concentration of 70% -90% is used for eluting, the elution volume of water for removing impurities is 5-BV 15, the elution volume of ethanol water solution for removing impurities is 10-20 BV, the elution volume of ethanol water solution for eluting a target component is 10-20 BV, ethanol water solution eluent with the volume concentration of 70% -90% is collected, and the crude extract of the stem and leaf of the paris polyphylla is obtained after concentration and drying.
4. The method for separating and preparing the high-purity saponin compound from the stem and leaf of the paris polyphylla as claimed in claim 1, wherein in step S3, the crude extract of the stem and leaf of the paris polyphylla is ultrasonically dissolved by using an acetonitrile aqueous solution with the volume concentration of 20-40%, then the crude extract is centrifuged at the rotating speed of 5000-15000 r/min, and the precipitate is taken to obtain the extract of the stem and leaf of the paris polyphylla.
5. The method for separating and preparing high-purity saponin compounds from the stems and leaves of the paris polyphylla as claimed in claim 1, wherein in step S4, the parameters of the preparation liquid chromatography are as follows:
chromatographic column Waters X Bridge prep C18OBD column (19 × 150mm, 5 μm);
mobile phase: the phase A is acetonitrile, the phase B is water, 0-24 min and 30-65% of acetonitrile; 24-27 min, 65% -95% acetonitrile; 27-35 min, 95% acetonitrile;
the flow rate is 15m L/min;
detection wavelength: and 203nm, and respectively receiving the target fraction I and the target fraction II according to the detection map.
6. The method for separating and preparing the high-purity saponin compound from the stems and leaves of the paris polyphylla as claimed in claim 1, wherein the purities of the paris polyphylla saponin II and the dioscin are respectively more than 95%.
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| CN112168912A (en) * | 2020-09-30 | 2021-01-05 | 云南贝泰妮生物科技集团股份有限公司 | Plant compound capable of inhibiting acne-related pathogenic bacteria and application thereof |
| CN115399345A (en) * | 2022-09-16 | 2022-11-29 | 西南林业大学 | Composition containing rhizoma paridis extract, and preparation method and application thereof |
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| CN101904968A (en) * | 2010-07-27 | 2010-12-08 | 天津大学 | Preparation method of Chinese paris rhizome yam type saponin and anti-tumor medicinal preparation thereof |
| CN109212111A (en) * | 2018-08-23 | 2019-01-15 | 广东东阳光药业有限公司 | Obtain the method and its application of Paris polyphylla extracting solution |
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| CN101693035A (en) * | 2009-10-15 | 2010-04-14 | 天津大学 | Medicinal preparation with inhibiting effect on tumor metastasis |
| CN101904968A (en) * | 2010-07-27 | 2010-12-08 | 天津大学 | Preparation method of Chinese paris rhizome yam type saponin and anti-tumor medicinal preparation thereof |
| CN109212111A (en) * | 2018-08-23 | 2019-01-15 | 广东东阳光药业有限公司 | Obtain the method and its application of Paris polyphylla extracting solution |
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| CN112168912A (en) * | 2020-09-30 | 2021-01-05 | 云南贝泰妮生物科技集团股份有限公司 | Plant compound capable of inhibiting acne-related pathogenic bacteria and application thereof |
| CN115399345A (en) * | 2022-09-16 | 2022-11-29 | 西南林业大学 | Composition containing rhizoma paridis extract, and preparation method and application thereof |
| CN115399345B (en) * | 2022-09-16 | 2024-01-26 | 西南林业大学 | Composition containing paris polyphylla extract and preparation method and application thereof |
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Application publication date: 20200728 |
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