CN110559328B - A method for preparing total saponins of herba Herminii with 11 ginsenosides as fingerprint characteristic components - Google Patents
A method for preparing total saponins of herba Herminii with 11 ginsenosides as fingerprint characteristic components Download PDFInfo
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Abstract
The invention relates to the technical field of extraction of effective components of traditional Chinese medicinal materials, in particular to a preparation method of total saponins of ginseng fruit by taking 11 ginsenosides as fingerprint characteristic components. The invention selects the buffer solution of citric acid and sodium citrate as the pH value regulator, accurately controls the pH value in the whole extraction process to be between 5.2 and 5.5, and ensures the pH value of the extracting solution to be stable in the whole extraction process. Preparing an extracting solution; adsorbing with macroporous resin, centrifuging at high speed, and spray drying to obtain total saponin powder of herba Herminii. During the process of extracting the ginseng fruit, the' prototype ginsenosides such as ginsenoside Re, Rg1, Rf, Rb1, Rb2 and the like are extracted, meanwhile, certain rare ginsenosides are generated, the types of the ginsenoside components contained in the ginseng fruit total saponins are improved, the ginseng fruit total saponins with 11 ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2 and Rg3 as fingerprint characteristic components are prepared, and the similarity of the ginseng fruit total saponins in each batch is ensured to be more than 0.97.
Description
Technical Field
The invention relates to the field of traditional Chinese medicines, in particular to a preparation method of total saponins of panax ginseng fruits by taking 11 ginsenosides as fingerprint characteristic components.
Background
In the prior art, ginseng (Panax ginseng c.a. Meyer) is a perennial herb of Panax of araliaceae, is mostly prepared from underground rhizomes, is sweet and slightly bitter in taste and slightly warm in nature, has the effects of greatly tonifying primordial qi, recovering pulse, solidifying collapse, tonifying spleen, benefiting lung, promoting fluid production, nourishing blood, soothing nerves, benefiting intelligence and the like, and is mainly used for treating diseases such as weak body, desire collapse, limb cold, pulse, spleen deficiency, anorexia, lung deficiency, cough and asthma, body fluid deficiency, thirst, internal heat, thirst, deficiency of both qi and blood, deficiency of weakness caused by long-term illness, palpitation, insomnia, impotence and the like. The ginseng is one of important special products in China, is also a rare medicinal material running in China and abroad, is known as 'all grass king' and has the effective components of saponins and polysaccharides, and modern researches show that the saponins in the ginseng have obvious pharmacological activities of resisting tumors, resisting diabetes, resisting cardiovascular and cerebrovascular diseases, resisting inflammation, resisting epilepsy, resisting oxidation and the like.
The ginseng fruit is a mature fruit of ginseng. As early as "supplement from compendium of materia Medica" there is a record of the drug. The initial fruit is green and bright red after ripening. The ginseng fruits are rare and precious because the ginseng fruits are not discarded but only one ginseng is discarded. According to systematic modern pharmaceutical research, Chinese scientists find that the ginseng fruit contains various substances such as saponin, polysaccharide, protein, amino acid and the like, and the effective components of the ginseng fruit are ginsenoside substances. The ginseng fruit contains more than 20 percent of total ginsenoside, which is 4 times of the root content of ginseng and is at the head of each part of ginseng plant. Based on the definite pharmacological activity of ginsenoside substances, ginseng fruits are used as raw material medicines to prepare various medicines for clinical application.
Ginsenoside belongs to tetracyclic triterpenoids, and can be classified into three types according to the structure of aglycon part, i.e. Protopanaxadiol type saponin (PPD), such as ginsenoside Ra1, Ra2, Rb1, Rb2, Rb3, Rc, Rg3, F2 and Rd; protopanaxatriol type saponin (PPT for short), such as ginsenoside Re, Rg1, Rf, Rg2, F1, F3 and Rh 1; oleanolic acid (Oleanolic acid) type saponins, such as ginsenoside Ro. The secondary metabolic derivative of the converted ginsenoside has stronger biological activity. This secondary metabolic derivative is named "rare ginsenoside", and the ginsenoside directly extracted from Araliaceae plants is called "prototype ginsenoside". At present, more than 60 rare ginsenosides have been discovered, including many rare ginsenosides with different anticancer activities such as Rk2, Rg3, Rh2, Rg5, Rh1, Rh3, Rk1, F1, F2, F3, etc. Since rare ginsenosides are secondary metabolites of ginsenosides, and are contained in very low amounts in ginseng extracts, these saponins can only be obtained by means such as chemical reactions, biotransformations, and the like.
The method comprises the steps of preparing a ginseng fruit total saponin fingerprint determination method by taking 11 ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2 and Rg3 as fingerprint characteristic components through vibration source capsule standardization research in 2018, determining 10 batches of ginseng fruit total saponins by using the fingerprint determination method, finding that the similarity of 10 batches of ginseng fruit total saponins is between 0.82 and 0.91, indicating that the batch-to-batch differences are large, finding out that the main reason is caused by the difference of pH value control in the extraction process of different batches of ginseng fruit total saponins through analysis, innovatively improving the preparation method of ginseng fruit total saponins, researching a full-automatic online citric acid-sodium citrate buffer solution pH value control system, and determining the optimal pH value control range in the extraction process, the 30 batches of the ginseng fruit total saponins are prepared according to the preparation method, the similarity of the 30 batches of the ginseng fruit total saponins is more than 0.97, and the stability and controllability of the quality of the ginseng fruit total saponins are ensured.
Disclosure of Invention
The invention provides a preparation method of total saponins of panax ginseng fruit by taking 11 ginsenosides as fingerprint characteristic components, which effectively controls the pH value in the whole extraction process to be between 5.2 and 5.5, ensures the pH value of the extracting solution to be stable in the whole extraction process, and effectively extracts rare ginsenosides of panax ginseng.
The technical scheme of the invention is as follows: a method for preparing total saponins of ginseng fruit by taking 11 ginsenosides as fingerprint characteristic components takes ginseng fruit as raw material, and is characterized by comprising the following steps:
(1) removing seeds and grinding the pulp: adding water into fresh herba Herminii, grinding into a pulp grinder to separate out semen Ginseng and pulp, collecting pulp, and refrigerating;
(2) full-automatic online citric acid-sodium citrate buffer solution pH value control system-hot reflux extraction: placing fresh pulp of herba Herminii in a hot reflux extraction tank equipped with a full-automatic online pH control system, adding water in an amount 2-5 times of the volume of the input materials, automatically measuring pH of the extractive solution with DG160 online pH detector in the full-automatic online citric acid-sodium citrate buffer solution pH control system, automatically adding citric acid-sodium citrate buffer solution to adjust pH to 5.2-5.5, heating to 100 deg.C, adding steam generated by heating water as new solvent, refluxing into the extraction tank, stirring, continuously extracting for 1 hr, monitoring pH of the extractive solution with DG160 online pH detector, adjusting pH to 5.2-5.5 with citric acid-sodium citrate buffer solution when the pH deviates from pH5.2-5.5, cooling, filtering, obtaining an extracting solution; standby;
(3) macroporous resin adsorption, namely taking clear filtrate obtained after the ginseng fruit extracting solution is filtered, adsorbing ginseng fruit saponin in the filtrate through a D101 macroporous resin column, saturating the filtrate, and washing the D101 macroporous resin column which adsorbs the liquid medicine with drinking water until effluent is nearly colorless; eluting the washed D101 macroporous resin column with 80% ethanol, and collecting ethanol eluate; and (3) concentrating under reduced pressure: introducing the ethanol eluent into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no ethanol smell exists, and concentrating under reduced pressure until the relative density is 1.05-1.20 and the temperature is 70 ℃;
(4) and (3) high-speed centrifugal spray drying, namely performing spray drying on the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to be 177-187 ℃, and collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, wherein the air inlet temperature is 15-25 r/min.
The preparation method comprises the following steps: compared with the original preparation process, the creativity of the preparation process lies in the step (2), the original preparation process only adds water for heating and extraction, and the pH value in the whole extraction process is not monitored and controlled. And (2) applying a full-automatic online citric acid-sodium citrate buffer solution pH value control system, using the citric acid-sodium citrate buffer solution as a pH value regulator, accurately controlling the pH value in the whole extraction process to be between 5.2 and 5.5, ensuring the pH value of an extracting solution in the whole extraction process to be stable, preparing the total ginsenoside with 11 ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2 and Rg3 as fingerprint characteristic components, and enabling the similarity of the prepared total ginsenosides to reach more than 0.97.
Compared with the ginsenoside acid hydrolysis method, the preparation method provided by the invention comprises the following steps: the acid used in the traditional acid hydrolysis method is inorganic acid or organic acid, the acid hydrolysis reaction is carried out in organic solvent or aqueous solution, the acid concentration is generally 1% -50%, the acid solution is mostly added into the raw materials at one time during the acid hydrolysis reaction of the ginsenoside, and the ginsenoside Re, Rg1, Rf, Rb1, Rb2 and other prototype ginsenosides are all hydrolyzed to generate rare ginsenoside. The embodiment proves that the content of the total saponins of the ginseng fruit can cause excessive decomposition of the ginsenoside Re and other prototype ginsenosides Rg1, Rf, Rb1, Rb2 and the like which are marked components of the total saponins of the ginseng fruit at the pH value of below 5.0, thereby causing the content to be reduced and further causing the similarity to be too low.
We find that the pH value of the extracting solution is between 5.0 and 5.8 after the ginseng fruit pulp is added with water through automatic pH value monitoring, and the pH value can be reduced to between 4.5 and 5.5 in the extracting process due to the influence of factors such as heating and the like, but the preparation method provided by the invention monitors and adjusts and controls the pH value to be within the range of 5.2 to 5.5 through a full-automatic online citric acid-sodium citrate buffer solution pH value control system, and in the pH value range, the prototype ginsenosides such as ginsenoside Re, Rg1, Rf, Rb1, Rb2 and the like can be properly decomposed to produce rare ginsenosides, the stability of the ginseng fruit total saponins among batches can be ensured, and the similarity of the ginseng fruit saponins can be ensured to be more than 0.97.
In the preparation method provided by the invention, the citric acid-sodium citrate buffer solution (with the pH value of 3.0-6.2) is selected from the aspects of safety, edibility and pH value of the buffer solution, and the citric acid is an organic acid, is safe and nontoxic and can be widely applied to the industries of food, medicine, daily chemicals and the like. The sodium citrate is sodium citrate, and is safe and nontoxic. By adjusting the dosage of citric acid and sodium citrate, a buffer solution with the pH value of 3.0-6.2 can be prepared.
Finger print detection of total ginsenoside of ginseng fruit with 11 ginsenosides as finger print characteristic components
[ fingerprinting ] chromatographic conditions and System suitability test chromatographic column: luna Omega Polar C18 (250 mm x 4.6mm,5 μm); mobile phase: acetonitrile (a) -0.2% phosphoric acid water (B), gradient elution is given in the table below; flow rate: 1.0 mL/min; detection wavelength: 203 nm; column temperature: 35 ℃; sample introduction amount: 10 muL. The elution time was 60 min. The chromatographic peak separation degree of 11 ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2 and Rg3 is more than 1.5.
[ preparation of reference solution ] precisely weighing 11 kinds of ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2, and Rg3, dissolving in 50ml of methanol solution, diluting to constant volume, and placing in a refrigerator at 4 deg.C to obtain the final product.
[ preparation of test solution ] about 20mg of powder of total saponins of Panax ginseng C.A. Meyer is taken, precisely weighed, and placed in a 50ml conical flask. Precisely adding 20ml of methanol, weighing, performing ultrasonic treatment for 30min, complementing the lost weight, uniformly mixing, and filtering with a 0.22-micron filter membrane.
[ MEASUREMENT METHOD ] precisely absorbing 10 muL of each of a reference solution and a sample solution, respectively, injecting into a liquid chromatograph, measuring, and recording a chromatogram to obtain the test solution.
The test sample characteristic peak atlas should have 11 characteristic peaks, the retention time of the corresponding reference substance peak should be the same, and the corresponding retention time should be within + -5% of the retention time of the reference substance peak. And according to the similarity evaluation system of the chromatographic fingerprint of the traditional Chinese medicine, the similarity of the fingerprint of the ginseng fruit total saponin sample and the fingerprint of the reference fingerprint is calculated through similarity.
The preparation method of the invention takes ginseng fruit as raw material, uses a full-automatic online citric acid-sodium citrate buffer solution pH value control system, selects safe, non-toxic and edible citric acid and sodium citrate buffer solution as pH value regulator, accurately controls the pH value in the whole extraction process to be between 5.2 and 5.5, ensures the pH value of the extracting solution to be stable in the whole extraction process, during the process of extracting the ginseng fruit, the' prototype ginsenosides such as ginsenoside Re, Rg1, Rf, Rb1, Rb2 and the like are extracted, meanwhile, certain rare ginsenosides are generated, the types of the ginsenoside components contained in the ginseng fruit total saponins are improved, the ginseng fruit total saponins with 11 ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2 and Rg3 as fingerprint characteristic components are prepared, and the similarity of the ginseng fruit total saponins in each batch is ensured to be more than 0.97.
The invention has the advantages that: 1. the method is characterized in that the ginseng fruit is used as a raw material, a full-automatic online citric acid-sodium citrate buffer solution pH value control system is adopted, safe, non-toxic and edible citric acid and sodium citrate buffer solution is selected as a pH value regulator, the pH value in the whole extraction process is accurately controlled to be between 5.2 and 5.5, the pH value of an extracting solution in the whole extraction process is ensured to be stable, the ginseng saponin Re, Rg1, Rf, Rb1, Rb2 and other 'prototype ginseng saponins' are extracted in the ginseng fruit extraction process, meanwhile, certain rare ginseng saponins are generated, the variety of the ginseng fruit total saponins containing ginseng saponin components is improved, 11 ginseng saponins Re, Rb1, F3, 2 Rg, Rc, Rb2, Rb3, F1, Rd, F2 and Rb3 are prepared as fingerprint characteristic components, and the similarity of the ginseng fruit total ginseng saponins in each batch is ensured to be more than 0.97. 2. The preparation method has advanced process technology, and the quality detection technology of the fingerprint spectrum using 11 ginsenosides as fingerprint characteristic components ensures the stability and controllability of the quality of the produced ginseng fruit total saponins, thereby ensuring the safety, effectiveness and controllability of clinical medication.
Drawings
FIG. 1: a full-automatic online pH value control system for citric acid-sodium citrate buffer solution.
FIG. 2: is a fingerprint spectrum of the total saponins of the ginseng fruit.
FIG. 3: 30 batches of ginseng fruit total saponin fingerprints prepared by the preparation method are provided.
Detailed Description
Referring to fig. 1, the parts are numbered as follows: a stirrer 1, a pH value electrode 2, a controller 3 and a citric acid-sodium citrate buffer solution 4.
Referring to fig. 2, peak 1: ginsenoside Re; peak 2: ginsenoside Rb 1; peak 3: ginsenoside F3; peak 4: ginsenoside Rg 2; peak 5: ginsenoside Rc; peak 6: ginsenoside Rb 2; peak 7: ginsenoside Rb 3; peak 8: ginsenoside F1; peak 9: ginsenoside Rd; peak 10: ginsenoside F2; peak 11: ginsenoside Rg 3.
Example 1
A process for preparing the general saponin of ginseng fruit with 11 ginsenosides as fingerprint features that 100 kg of fresh ginseng fruit is mixed with 20 kg of water and then ground in a grinder to separate out ginseng seed and pulp, which are then collected. Placing fresh pulp of ginseng fruit in a hot reflux extraction tank provided with a full-automatic online citric acid-sodium citrate buffer solution pH value control system, adding 100 kg of water, automatically adding citric acid-sodium citrate buffer solution through the system to adjust the pH value of an extracting solution to be 5.3, heating to 100 ℃, continuously extracting for 1 hour, cooling, filtering, taking a filtered clear filtrate, adsorbing ginseng fruit saponin by a D101 macroporous resin column, saturating, washing the D101 macroporous resin column adsorbing the liquid medicine with drinking water until an effluent liquid is nearly colorless, eluting the washed D101 macroporous resin column with 80% ethanol, and collecting ethanol eluent. Introducing the ethanol eluate into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no alcohol smell is produced, and concentrating under reduced pressure until the relative density is 1.10 (70 deg.C). And (3) spray-drying the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to be 177-187 ℃, and collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, wherein the air inlet temperature is 15-25 r/min.
Example 2
A process for preparing the general saponin of ginseng fruit with 11 ginsenosides as fingerprint features that 100 kg of fresh ginseng fruit is mixed with 20 kg of water and then ground in a grinder to separate out ginseng seed and pulp, which are then collected. Placing fresh pulp of ginseng fruit in a hot reflux extraction tank provided with a full-automatic online citric acid-sodium citrate buffer solution pH value control system, adding 100 kg of water, automatically adding citric acid-sodium citrate buffer solution through the system to adjust the pH value of an extracting solution to be pH5.4, heating to 100 ℃, returning steam generated by heating water to an extractor as a new solvent, continuously extracting for 1 hour, cooling, filtering, taking a filtered clear filtrate, adsorbing ginseng fruit saponin by a D101 macroporous resin column, adsorbing saturation, washing the D101 macroporous resin column adsorbing the liquid medicine with drinking water until an effluent liquid is nearly colorless, eluting the D101 macroporous resin column washing with water with 80% ethanol, and collecting ethanol eluent. Introducing the ethanol eluate into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no alcohol smell is produced, and concentrating under reduced pressure until the relative density is 1.10 (70 deg.C). And (3) spray-drying the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to be 177-187 ℃, and collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, wherein the air inlet temperature is 15-25 r/min.
15 batches of the total saponins of panax ginseng are produced respectively according to the preparation methods of the above examples 1 and 2, and 30 batches of total saponins of panax ginseng are obtained. The 30 batches of the ginseng fruit total saponins are measured according to a fingerprint spectrum measuring method taking 11 ginsenosides as fingerprint characteristic components, 11 ginseng saponin component characteristic peaks exist in a sample fingerprint spectrum, the retention time of the sample fingerprint spectrum is the same with that of corresponding reference substance peaks, according to a traditional Chinese medicine chromatogram fingerprint spectrum similarity evaluation system, the similarity of the 30 batches of the ginseng fruit total saponin fingerprint spectrum and a comparison fingerprint spectrum is calculated through the similarity, the similarity is all over 0.97, and the specific result is shown in table 1, and is shown in figure 2 and figure 3.
Example 3
A process for preparing the general saponin of ginseng fruit with 11 ginsenosides as fingerprint features that 100 kg of fresh ginseng fruit is mixed with 20 kg of water and then ground in a grinder to separate out ginseng seed and pulp, which are then collected. Placing fresh pulp of ginseng fruit into a hot reflux extraction tank provided with a full-automatic online citric acid-sodium citrate buffer solution pH value control system, adding 100 kg of water, automatically adding citric acid-sodium citrate buffer solution through the system to adjust the pH value of an extracting solution to be pH5.0, heating to 100 ℃, continuously extracting for 1 hour, cooling, filtering, taking a filtered clear filtrate, adsorbing ginseng fruit saponin by a D101 macroporous resin column, saturating, washing the D101 macroporous resin column which adsorbs the liquid medicine with drinking water until an effluent liquid is nearly colorless, eluting the washed D101 macroporous resin column with 80% ethanol, and collecting ethanol eluent. Introducing the ethanol eluate into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no alcohol smell is produced, and concentrating under reduced pressure until the relative density is 1.10 (70 deg.C). Spray drying the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to 177-187 ℃, and rotating at 15-25 r/min, collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, and producing 2 batches of products according to the example 3, wherein the specific results are shown in Table 1.
Example 4
A process for preparing the general saponin of ginseng fruit with 11 ginsenosides as fingerprint features that 100 kg of fresh ginseng fruit is mixed with 20 kg of water and then ground in a grinder to separate out ginseng seed and pulp, which are then collected. Placing fresh pulp of ginseng fruit into a hot reflux extraction tank equipped with a full-automatic online citric acid-sodium citrate buffer solution pH value control system, adding 100 kg of water, automatically adding citric acid-sodium citrate buffer solution through the system to adjust the pH value of an extracting solution to be 4.5, heating to 100 ℃, continuously extracting for 1 hour, cooling, filtering, taking a filtered clear filtrate, adsorbing ginseng fruit saponin by a D101 macroporous resin column, saturating, washing the D101 macroporous resin column which adsorbs the liquid medicine with drinking water until an effluent liquid is nearly colorless, eluting the washed D101 macroporous resin column with 80% ethanol, and collecting ethanol eluent. Introducing the ethanol eluate into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no alcohol smell is produced, and concentrating under reduced pressure until the relative density is 1.10 (70 deg.C). Spray drying the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to 177-187 ℃, and rotating at 15-25 r/min, collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, and producing 2 batches of products according to the above example 4, wherein the specific results are shown in Table 1.
Example 5
A process for preparing the general saponin of ginseng fruit with 11 ginsenosides as fingerprint features that 100 kg of fresh ginseng fruit is mixed with 20 kg of water and then ground in a grinder to separate out ginseng seed and pulp, which are then collected. Placing fresh pulp of ginseng fruit into a hot reflux extraction tank equipped with a full-automatic online citric acid-sodium citrate buffer solution pH value control system, adding 100 kg of water, automatically adding citric acid-sodium citrate buffer solution through the system to adjust the pH value of an extracting solution to be 4.0, heating to 100 ℃, continuously extracting for 1 hour, cooling, filtering, taking a filtered clear filtrate, adsorbing ginseng fruit saponin by a D101 macroporous resin column, saturating, washing the D101 macroporous resin column which adsorbs the liquid medicine with drinking water until an effluent liquid is nearly colorless, eluting the washed D101 macroporous resin column with 80% ethanol, and collecting ethanol eluent. Introducing the ethanol eluate into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no alcohol smell is produced, and concentrating under reduced pressure until the relative density is 1.10 (70 deg.C). Spray drying the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to 177-187 ℃, and rotating at 15-25 r/min, collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, and producing 2 batches of products according to the example 5, wherein the specific results are shown in Table 1.
Example 6
100 kg of fresh ginseng fruit is taken, 20 kg of water is added, the fresh ginseng fruit is put into a pulping machine to separate ginseng seeds and pulp, and the pulp is collected. Placing fresh ginseng fruit pulp into a hot reflux extraction tank, adding 100 kg of water, heating to 100 ℃ without monitoring the pH value, continuously extracting for 1 hour, cooling, filtering, taking the filtered clear filtrate, adsorbing ginseng fruit saponin by using a D101 macroporous resin column, saturating the filtrate by adsorption, washing the D101 macroporous resin column which adsorbs the liquid medicine with drinking water until the effluent liquid is nearly colorless, eluting the D101 macroporous resin column which is washed with water with 70% ethanol, and collecting ethanol eluent. Introducing the ethanol eluate into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no alcohol smell is produced, and concentrating under reduced pressure until the relative density is 1.10 (70 deg.C). Spray drying the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to 177-187 ℃, and rotating at 15-25 r/min, collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder, and producing 2 batches of products according to the example 6, wherein the specific results are shown in Table 1.
Example 7, the total saponins of panax ginseng obtained in example 6 were subjected to fingerprint analysis by a fingerprint analysis method using 11 ginsenosides as fingerprint characterizing components, and the similarity between the fingerprint of the total saponins of panax ginseng obtained in example 6 and the reference fingerprint was calculated to be less than 0.90 according to a traditional Chinese medicine chromatogram fingerprint similarity evaluation system.
Note: 1-10: 10 batches produced for the original standard preparation process.
Examples 1-1 to 1-15: 15 samples of example 1 produced according to the preparation process of the present invention.
2-1 to 2-15: 15 samples of example 2 produced according to the preparation process of the present invention.
Examples 3-1, 3-2: 2 samples of example 3.
Seed 4-1, seed 4-2: 2 samples of example 4.
Fruit 5-1, fruit 5-2: 2 samples of example 5.
Seed 6-1, seed 6-2: 2 samples of example 6.
From the above table, the effect of pH on similarity can be seen.
The foregoing description is only exemplary of the invention and is not intended to limit the spirit of the invention.
Claims (1)
1. A method for preparing total saponins of ginseng fruit by taking 11 ginsenosides as fingerprint characteristic components takes ginseng fruit as raw material, and is characterized by comprising the following steps:
(1) removing seeds and grinding the pulp: adding water into fresh herba Herminii, grinding into a pulp grinder to separate out semen Ginseng and pulp, collecting pulp, and refrigerating;
(2) full-automatic online citric acid-sodium citrate buffer solution pH value control system-hot reflux extraction: placing fresh pulp of herba Herminii in a hot reflux extraction tank equipped with a full-automatic online pH control system, adding water in an amount 2-5 times of the volume of the input materials, automatically measuring pH of the extractive solution with DG160 online pH detector in the full-automatic online citric acid-sodium citrate buffer solution pH control system, automatically adding citric acid-sodium citrate buffer solution to adjust pH to 5.2-5.5, heating to 100 deg.C, adding steam generated by heating water as new solvent, refluxing into the extraction tank, stirring, continuously extracting for 1 hr, monitoring pH of the extractive solution with DG160 online pH detector, adjusting pH to 5.2-5.5 with citric acid-sodium citrate buffer solution when the pH deviates from pH5.2-5.5, cooling, filtering, obtaining an extracting solution; standby;
(3) macroporous resin adsorption, namely taking clear filtrate obtained after the ginseng fruit extracting solution is filtered, adsorbing ginseng fruit saponin in the filtrate through a D101 macroporous resin column, saturating the filtrate, and washing the D101 macroporous resin column which adsorbs the liquid medicine with drinking water until effluent is nearly colorless; eluting the washed D101 macroporous resin column with 80% ethanol, and collecting ethanol eluate; and (3) concentrating under reduced pressure: introducing the ethanol eluent into an external circulation single-effect concentrator, recovering ethanol under reduced pressure until no ethanol smell exists, and concentrating under reduced pressure until the relative density is 1.05-1.20 and the temperature is 70 ℃;
(4) high-speed centrifugal spray drying, namely performing spray drying on the concentrated solution by using a high-speed centrifugal spray dryer, controlling the air inlet temperature to be 177-187 ℃, and collecting medicinal powder in a D-level clean area to obtain the ginseng fruit total saponin powder;
the prepared total saponins of ginseng fruit with 11 ginsenosides Re, Rb1, F3, Rg2, Rc, Rb2, Rb3, F1, Rd, F2 and Rg3 as fingerprint characteristic components has a similarity of more than 0.97.
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| CN101966292A (en) * | 2010-10-07 | 2011-02-09 | 吉林省集安益盛药业股份有限公司 | Sugarless Chinese medicinal oral liquid and preparation method thereof |
| CN105999278A (en) * | 2016-05-24 | 2016-10-12 | 成都市斯贝佳科技有限公司 | Injecting medicine composition for improving stability of ginsenoside medicine injection |
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| CN101966292A (en) * | 2010-10-07 | 2011-02-09 | 吉林省集安益盛药业股份有限公司 | Sugarless Chinese medicinal oral liquid and preparation method thereof |
| CN105999278A (en) * | 2016-05-24 | 2016-10-12 | 成都市斯贝佳科技有限公司 | Injecting medicine composition for improving stability of ginsenoside medicine injection |
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