CN113045614A - Method for simultaneously separating and purifying multiple flavonoids by using industrial chromatographic technology - Google Patents
Method for simultaneously separating and purifying multiple flavonoids by using industrial chromatographic technology Download PDFInfo
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- 229930003935 flavonoid Natural products 0.000 title claims abstract description 11
- 235000017173 flavonoids Nutrition 0.000 title claims abstract description 11
- 150000002215 flavonoids Chemical class 0.000 title claims abstract description 10
- 238000005516 engineering process Methods 0.000 title claims description 8
- RPMNUQRUHXIGHK-PYXJVEIZSA-N apigenin 7-O-neohesperidoside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=C2C(=O)C=C(C=3C=CC(O)=CC=3)OC2=C1 RPMNUQRUHXIGHK-PYXJVEIZSA-N 0.000 claims abstract description 38
- 229930034861 apigenin-7-O-neohesperidoside Natural products 0.000 claims abstract description 38
- RPMNUQRUHXIGHK-SBDOOABHSA-N rhoifolin Natural products O([C@@H]1[C@@H](O)[C@H](O)[C@H](CO)O[C@H]1Oc1cc(O)c2C(=O)C=C(c3ccc(O)cc3)Oc2c1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@H](C)O1 RPMNUQRUHXIGHK-SBDOOABHSA-N 0.000 claims abstract description 38
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- 241001530028 Turpinia formosana Species 0.000 claims description 17
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- IQVQXVFMNOFTMU-FLIBITNWSA-N (Z)-ligustilide Chemical compound C1CC=CC2=C1C(=C/CCC)/OC2=O IQVQXVFMNOFTMU-FLIBITNWSA-N 0.000 claims description 11
- IQVQXVFMNOFTMU-DHZHZOJOSA-N Z-ligustilide Natural products C1CC=CC2=C1C(=C/CCC)\OC2=O IQVQXVFMNOFTMU-DHZHZOJOSA-N 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 239000012488 sample solution Substances 0.000 claims description 10
- 239000003480 eluent Substances 0.000 claims description 9
- 239000000523 sample Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000010828 elution Methods 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229920003053 polystyrene-divinylbenzene Polymers 0.000 claims description 2
- ZOLPMMWNCLHKPX-UHFFFAOYSA-N ligustrin Natural products CC1=CCC2C1C3OC(=C)C(=O)C3C(O)CC2=C ZOLPMMWNCLHKPX-UHFFFAOYSA-N 0.000 abstract description 19
- QJVXKWHHAMZTBY-GCPOEHJPSA-N syringin Chemical compound COC1=CC(\C=C\CO)=CC(OC)=C1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 QJVXKWHHAMZTBY-GCPOEHJPSA-N 0.000 abstract description 19
- 238000002360 preparation method Methods 0.000 abstract description 17
- 239000013558 reference substance Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 7
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- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000178 monomer Substances 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 7
- 238000010992 reflux Methods 0.000 description 7
- 241001436151 Turpinia arguta Species 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 241000830535 Ligustrum lucidum Species 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 3
- -1 flavonoid glycoside compound Chemical class 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 238000004237 preparative chromatography Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FINHMKGKINIASC-UHFFFAOYSA-N Tetramethylpyrazine Chemical compound CC1=NC(C)=C(C)N=C1C FINHMKGKINIASC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 239000001606 7-[(2S,3R,4S,5S,6R)-4,5-dihydroxy-6-(hydroxymethyl)-3-[(2S,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxyoxan-2-yl]oxy-5-hydroxy-2-(4-hydroxyphenyl)chroman-4-one Substances 0.000 description 1
- 102000005348 Neuraminidase Human genes 0.000 description 1
- 108010006232 Neuraminidase Proteins 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 108010093894 Xanthine oxidase Proteins 0.000 description 1
- 102100033220 Xanthine oxidase Human genes 0.000 description 1
- 230000003276 anti-hypertensive effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 235000013399 edible fruits Nutrition 0.000 description 1
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- DFPMSGMNTNDNHN-ZPHOTFPESA-N naringin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC=2C=C3O[C@@H](CC(=O)C3=C(O)C=2)C=2C=CC(O)=CC=2)O[C@H](CO)[C@@H](O)[C@@H]1O DFPMSGMNTNDNHN-ZPHOTFPESA-N 0.000 description 1
- 229930019673 naringin Natural products 0.000 description 1
- 229940052490 naringin Drugs 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 241000712461 unidentified influenza virus Species 0.000 description 1
- 230000029812 viral genome replication Effects 0.000 description 1
- 230000009385 viral infection Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
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Abstract
The invention discloses a method for simultaneously separating and purifying various flavonoids by utilizing an industrial chromatographic technique, wherein the purities of the monomers of the simultaneously prepared ligustrin and rhoifolin are both more than 99.5%; the method can realize real-time online monitoring of the separation process; the method has the advantages of good process reproducibility, simple operation, short preparation time, small organic solvent consumption, and suitability for large-scale industrial production, and can be used for simultaneously preparing two reference substances, so that the utilization rate of medicinal materials is improved, and the method is ecological-friendly.
Description
Technical Field
The invention belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines, and particularly relates to a method for simultaneously separating and purifying various flavonoid substances by utilizing an industrial chromatographic technique.
Background
Ligustrum lucidum is a flavonoid glycoside compound, is one of main active ingredients of fructus Ligustri Lucidi and folium Turpiniae, and has effects of inhibiting influenza virus infection and replication and inhibiting neuraminidase. Rhoifolin is flavonoid glycoside compound, is one of main active ingredients of leaves of Turpinia arguta and Rutaceae plant fruits (such as exocarpium Citri Grandis), and has antioxidant, antitumor, antihypertensive and xanthine oxidase inhibiting effects.
At present, ligustrin and rhoifolin reference substances are needed to be used for controlling the quality of medicinal materials, screening pharmacological and medicinal effects, developing new products and the like. However, the method is limited by the fact that the reference substance is few in source and difficult to separate and purify, the prices of the ligustilide and rhoifolin reference substances are relatively high, the number of ligustilide is 500 yuan/count, and the number of rhoifolin is 1200 yuan/count, and the quality control of medicinal materials containing the ligustilide and rhoifolin and related products thereof is severely limited. Therefore, the development of a method for simply and rapidly separating and purifying high-purity ligustrin and rhoifolin components at the same time is the focus of the current research.
The currently disclosed preparation methods for ligustrin and rhoifolin are both preparation of a single compound. For example, CN101899078A discloses a method for extracting ligustrin from folium Turpiniae or fructus Ligustri Lucidi, CN 102633850a discloses an extraction method of rhoifolin and its application in preparing medicine, CN 102286043a discloses a purification method of rhoifolin, CN 103833810a discloses a new technology for preparing rhoifolin, and CN 106632546A discloses a method for simultaneously preparing two chemical references of rhoifolin and naringin. By contrast, the method has the defects of small scale batch, long process steps, environmental pollution and the like, the reference substance cannot be prepared in large batch to meet the requirements of the current research, and a single reference substance is separated from the medicinal materials, so that the medicinal material resources are wasted, and the method is not beneficial to environmental protection and sustainable utilization.
CN 102579522A discloses an ethanol percolation extract of total flavonoids of turpinia arguta and a preparation method and application thereof, and CN 101862357A discloses an ethanol reflux extract of total flavonoids of turpinia arguta and a preparation method and application thereof, wherein the prepared extract mainly contains flavonoid compounds such as ligustrin, rhoifolin and the like. However, the prior art for simultaneously preparing the ligustilide and rhoifolin reference substances is not found.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for simultaneously separating, purifying and preparing various flavonoid substances by using an industrial chromatographic technique, in particular to a method for simultaneously preparing ligustrin and rhoifolin reference substances from turpinia formosana leaf extract by using an industrial chromatographic preparation technique, which realizes real-time online monitoring of the separation process and small organic solvent consumption; simple preparation process, short production period, easy industrialization, environmental protection and high purity.
The invention provides a method for preparing a flavonoid reference substance by using an industrial preparative chromatography purification technology, which comprises the following steps: injecting the solution of the folium Turpiniae extract sample into a high-pressure preparative chromatogram according to a certain sample amount, eluting with a solvent system 1, detecting the separation condition with an ultraviolet online detector, respectively collecting the eluates of the prepared monomeric compounds of the ligustilide and the rhoifolin according to the peak emergence time and the chromatographic peak height of the ligustilide and the rhoifolin, collecting the start and stop time respectively of 175 and 220 and 250min, and respectively concentrating and drying the eluates;
the flavonoid reference substances comprise ligustrin and rhoifolin;
preparing a turpinia formosana extract sample solution: taking the turpinia formosana leaf extract, adding a proper amount of solvent system 2 to dissolve the turpinia formosana leaf extract, preparing a sample solution with a certain concentration, and filtering for later use.
Preferably, the content of the ligustilide in the turpinia formosana leaf extract is 1.0-9.0% (W/W), preferably 2.0-8.0% (W/W); the content of rhoifolin is 0.5-7.0% (W/W), preferably 1.0-6.0% (W/W); and/or, the solvent system 2 is 5.0-15.0% (V/V) methanol aqueous solution; preferably 8.0% to 12.0% (V/V) methanol in water.
Preferably, the concentration of the sample solution is 50-100 mg/mL; preferably 70-90 mg/mL.
Preferably, the industrial preparative chromatographic packing is polystyrene-divinylbenzene polymer packing; CG161M or MCI GEL CHP20P is preferred.
Preferably, the solvent system 1 is one or more of methanol, water and trifluoroacetic acid; preferably a mixed solution of methanol, water and trifluoroacetic acid; more preferably the volume ratio of methanol, water and trifluoroacetic acid is 30-50:70-50:0.5, such as 40:60:0.5, 43:57:0.5 and 45:55: 0.5.
Preferably, the elution flow rate is 2.5-7.5 CV/h; preferably 2.5-5.0 CV/h;
preferably, the sample injection amount is 120-150L.
Preferably, the detection wavelength of the ultraviolet online detector is 336 nm.
Preferably, the concentration is concentration under reduced pressure; and/or the temperature of concentration is 50-60 ℃.
Preferably, the drying is vacuum drying; and/or the drying temperature is 40-50 ℃.
Preferably, the method for extracting the turpinia arguta leaves comprises the following steps: reflux-extracting appropriate amount of folium Turpiniae with ethanol for several times (such as 1, 2, 3 times, etc.), each time for 1-3 hr, and filtering; mixing filtrates, recovering ethanol from filtrate, adsorbing the water solution with nonpolar macroporous adsorbent resin, eluting with ethanol of less than 20% to remove impurities, eluting with 25-90% ethanol, collecting eluate, recovering ethanol, concentrating, and drying.
The invention has the beneficial technical effects that:
1. according to the invention, the turpinia formosana leaf extract is directly separated and purified by an industrial preparative chromatography, 2 reference substance compounds (ligustrin and rhoifolin) are obtained at the same time, the purity can reach more than 99.5%, and the problems of difficult preparation, high price and the like of the reference substance can be solved.
2. The method for preparing the reference substance simultaneously by using the industrial chromatographic preparation technology realizes real-time online monitoring of the separation process; the organic solvent consumption is less, the preparation process is simple, the production period is short, the industrialization is easy, the environment is friendly, and the like.
3. The invention adopts one medicinal material and prepares 2 reference compounds simultaneously, thereby improving the utilization rate of the medicinal material and saving the cost.
Drawings
FIG. 1: HPLC chromatogram of folium Turpiniae extract;
FIG. 2: a process flow chart for preparing ligustilide and rhoifolin;
FIG. 3: HPLC chromatogram of ligustrazine;
FIG. 4: HPLC chromatogram of rhoifolin;
Detailed Description
For a better understanding of the present invention, the technical solutions of the present invention are further described and illustrated by the following examples.
Example 1: preparation method of folium Turpiniae extract
Taking a proper amount of turpinia formosana leaves, adding 70% ethanol with the volume 10 times of the turpinia formosana leaves, performing reflux extraction for 2 times, performing reflux extraction for 1 hour each time, and filtering; mixing filtrates, recovering ethanol from filtrate, adsorbing water solution with nonpolar macroporous adsorbent resin, eluting with ethanol (such as 18%) below 20% to remove impurities, eluting with 70% ethanol, collecting eluate, recovering ethanol, concentrating, and drying to obtain folium Turpiniae extract with Ligustrum lucidum ait content of about 8.0% (W/W) and rhoifolin content of about 6.0% (W/W) as shown in figure 1.
Example 2: preparation method of folium Turpiniae extract
Taking a proper amount of turpinia formosana leaves, adding 30% ethanol with the volume 5 times of the turpinia formosana leaves, performing reflux extraction for 1 time, performing reflux extraction for 1 hour each time, and filtering; mixing filtrates, recovering ethanol from filtrate, adsorbing water solution with nonpolar macroporous adsorbent resin, eluting with ethanol (such as 15%) below 20% to remove impurities, eluting with 25% ethanol, collecting eluate, recovering ethanol, concentrating, and drying to obtain folium Turpiniae extract with Ligustrum lucidum ait content of about 2.0% (W/W) and rhoifolin content of about 1.0% (W/W).
Example 3: preparation method of folium Turpiniae extract
Taking a proper amount of turpinia formosana leaves, adding 90% ethanol with 15 times of volume, performing reflux extraction for 2 times, performing reflux extraction for 2 hours each time, and filtering; mixing filtrates, recovering ethanol from filtrate, adsorbing water solution with nonpolar macroporous adsorbent resin, eluting with ethanol (such as 10%) below 20% to remove impurities, eluting with 90% ethanol, collecting eluate, recovering ethanol, concentrating, and drying to obtain folium Turpiniae extract with Ligustrum lucidum ait content of about 6.0% (W/W) and rhoifolin content of about 3.0% (W/W).
Example 4: preparation of ligustrin and rhoifolin
A method for simultaneously preparing ligustrin and rhoifolin reference substances from folium Turpiniae extract by using industrial chromatographic preparation technology is shown in figure 2, and comprises the following steps:
(1) 10800g of the Turpinia arguta leaf extract of example 1 was dissolved by adding 12.0% (V/V) methanol aqueous solution and prepared into a sample solution with a concentration of 90mg/mL, and the sample solution was filtered for use.
(2) Injecting 120L of the sample liquid in the step (1) into an industrial preparative chromatograph, wherein the purification filler is CG161M, the methanol, the water and the trifluoroacetic acid solution (40:60:0.5, V/V/V) are used as eluent, the elution flow rate is 5.0CV/h, and the ultraviolet detection wavelength is 336 nn. Collecting the prepared eluates containing the ligustrin and the rhoifolin according to the peak emergence time and the chromatographic peak height of the ligustrin and the rhoifolin, respectively collecting the start and stop time of 175-200min and 220-250min, respectively, concentrating the eluates with high purification of the target components at 55 ℃ under reduced pressure until the eluates are dried at 45 ℃ and then drying in vacuum for 24h to obtain 691.21g of ligustrin with the purity of more than 99.5 percent (see figure 3), 518.45g of rhoifolin with the purity of more than 99.5 percent (see figure 4).
Example 5: preparation of ligustrin and rhoifolin
A method for simultaneously preparing ligustrin and rhoifolin reference substances from folium Turpiniae extract by using industrial chromatographic preparation technology is shown in figure 2, and comprises the following steps:
10500g of the Turpinia arguta leaf extract of example 2 was dissolved by adding 8.0% (V/V) methanol aqueous solution and prepared into a sample solution having a concentration of 70mg/mL, and the sample solution was filtered for use.
(2) Separation, purification and drying: injecting 150L of the sample liquid obtained in the step (1) into an industrial preparative chromatography, wherein the purified filler is MCI GEL CHP20P, methanol, water, trifluoroacetic acid solution (45:55:0.5, V/V/V) is used as an eluent, the elution flow rate is 2.5CV/h, the ultraviolet detection wavelength is 336nn, the prepared eluents containing the ligustrin and the rhoifolin are collected according to the peak emergence time and the chromatographic peak height of the ligustrin and the rhoifolin respectively, the collection starting and stopping times are respectively 175-220-180 min and 250-220-4 min, the eluents with the high purified target components are respectively subjected to vacuum concentration at 55 ℃ until the eluents are dried, and then the eluents are subjected to vacuum drying at 45 ℃ for 24h to obtain 178.36g of the ligustrin, the purity is more than 99.5%, and the rhoifolin is 89.25g, and the purity is more than 99.5%.
The above preferred embodiments are merely to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and the technical solution of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for simultaneously separating and purifying various flavonoids by using an industrial chromatographic technology comprises the following steps: injecting a solution of a turpinia formosana leaf extract sample into a high-pressure industrial preparative chromatogram according to a certain sample amount, eluting by using a solvent system 1, detecting the separation condition by using an ultraviolet online detector, respectively collecting eluents of prepared ligustilide and rhoifolin monomeric compounds according to the peak-yielding time and the chromatographic peak height of the ligustilide and the rhoifolin, collecting the eluents with the starting and stopping time of respectively 175 and 220 and 250min, and respectively concentrating and drying the eluents;
preparing a turpinia formosana extract sample solution: taking the turpinia formosana leaf extract, adding a proper amount of solvent system 2 to dissolve the turpinia formosana leaf extract, preparing a sample solution with a certain concentration, and filtering for later use.
2. The method according to claim 1, wherein the amount of ligustilide in the turpinia formosana leaf extract is 1.0-9.0% (W/W), preferably 2.0-8.0% (W/W); the content of rhoifolin is 0.5-7.0% (W/W), preferably 1.0-6.0% (W/W); and/or, the solvent system 2 is 5.0-15.0% (V/V) methanol aqueous solution; preferably 8.0% to 12.0% (V/V) methanol in water.
3. The method of claim 1, wherein the sample solution has a concentration of 50-100 mg/mL; preferably 70-90 mg/mL.
4. The method of claim 1, wherein the industrial chromatography packing is a polystyrene-divinylbenzene polymeric packing; CG161M or MCIGEL CHP20P is preferred.
5. The method of claim 1, the solvent system 1 is one or more of methanol, water, trifluoroacetic acid; preferably a mixed solution of methanol, water and trifluoroacetic acid; more preferably the volume ratio of methanol, water and trifluoroacetic acid is 30-50:70-50:0.5, such as 40:60:0.5, 43:57:0.5 and 45:55: 0.5.
6. The method of claim 1, wherein the elution flow rate is 2.5-7.5 CV/h; preferably 2.5-5.0 CV/h.
7. The method as claimed in claim 1, wherein the sample volume is 120-150L.
8. The method of claim 1, wherein the ultraviolet online detector has a detection wavelength of 336 nm.
9. The method of claim 1, the concentrating is concentrating under reduced pressure; and/or the temperature of concentration is 50-60 ℃, and/or the drying is vacuum drying; and/or the drying temperature is 40-50 ℃.
10. The method of claim 1, wherein the method for extracting turpinia formosana comprises: reflux-extracting appropriate amount of folium Turpiniae with ethanol for several times (such as 1, 2, 3 times, etc.), each time for 1-3 hr, and filtering; mixing filtrates, recovering ethanol from filtrate, adsorbing the water solution with nonpolar macroporous adsorbent resin, eluting with ethanol of less than 20% to remove impurities, eluting with 25-90% ethanol, collecting eluate, recovering ethanol, concentrating, and drying.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633850A (en) * | 2010-08-16 | 2012-08-15 | 江西山香药业有限公司 | Rhoifolin extraction method and usage of drug prepared by rhoifolin |
| CN102784178A (en) * | 2010-04-13 | 2012-11-21 | 江西山香药业有限公司 | Turpinia montana leaf general flavone ethanol reflux extractive, preparation method and application thereof |
| CN102920751A (en) * | 2010-04-13 | 2013-02-13 | 江西山香药业有限公司 | Turpinia arguta leaf total flavonoid ethanol reflux extract, preparation method and uses thereof |
| CN102935098A (en) * | 2010-04-13 | 2013-02-20 | 江西山香药业有限公司 | Acute turpinia leaf general flavone ethanol reflux extract, and preparation method and application thereof |
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