CN102579564B - Preparing method of Tibetan capillaris effective part extractives - Google Patents
Preparing method of Tibetan capillaris effective part extractives Download PDFInfo
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Abstract
The invention relates to a preparing method of Tibetan capillaris effective part extractives, which comprises the steps of drying, cutting Tibetan capillaries into 0.5 to 2 cm sections, subjecting the cut Tibetan capillaries to cold soak by adding pure water or ethanol solution, extracting the cold soaked Tibetan capillaries through ultrasound, filtering the capillaries through filter cloth, and obtaining the crude extract; obtaining centrifugate after the centrifuging and impurity-removing of the crude extract, removing the ethanol through the pressure reducing and concentration of the centrifugate, adding pure water to the volume dose before concentration, and obtaining the extract; subjecting the extract to purification and separation by using membrane separation method of ceramic membrane clarification and ultrafiltration membrane separation, and obtaining ultrafiltration separation liquid; absorbing the ultrafiltration separation liquid with macroporous resin, then eluting the absorbed ultrafitration separation liquid with ethanol solution, and obtaining eluent; concentrating the eluent through nanofiltration membrane to obtain concentrated liquid, drying the concentrated liquid to constant weight, and obtaining the Tibetan capillaris effective part extractives. The method has the advantages of being good in separating effect, high in yield, good in product quality, capable of achieving linear amplification, and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of plant extract, relate in particular to the preparation method of ZANGYINCHEN effective part extract.
Background technology
" ZANGYINCHEN " is to treat liver-gallbladder disease, hemopathic characteristic medicine resource plant in the Tibetan medicine medical science.The described ZANGYINCHEN of Tibetan medicine refers to Tibetan medicine " DIDA ", and " DIDA " is mainly several 10 kind of plant such as Swertia, Herba Haleniae Corniculatae genus, Herba Gentianopsis Paludosae genus and Lomatogonium rotatum (L) Fries ex Nym genus of Gentianaceae." ZANGYINCHEN " medical material contains iridoids and mouthful diphenylene ketone oxide constituents, is the main pharmacodynamics composition of hepatobiliary system diseases such as " ZANGYINCHEN " treatment hepatitis and cholecystitis.Chinese invention patent (the patent No.: 92108809.4) disclose a kind of production method of extraction process, equipment and ZANGYINCHEN tablet of ZANGYINCHEN effective ingredient, this method is a raw material with the ZANGYINCHEN grass, ethanol is extractant, continuously abstraction process production ZANGYINCHEN tablet; Chinese invention patent (the patent No.: 200710061832.4) disclose a kind of preparation technology of Tibet capilary artemisia, this technology is raw material with the ZANGYINCHEN, holds back the water injection and the freeze dried powder of the various hepatitis of method production for treating, cholecystitis, hepatic injury, hepatic fibrosis, fatty liver diseases through hydrophilic solvent extraction, Gravity Separation and molecular sieve; Chinese invention patent (patent No.: 200710061832.4) disclose a kind of by extraction, remove impurity, concentrate, initial gross separation, adsorbing separation, concentrate, dry, pulverize, the further ZANGYINCHEN extraction of effective components that forms of process equipment such as refining, this method adopts water, ethanol extraction, ethanol ultrasonic extraction adopts absorption, separating effective ingredients such as centrifugal, macroporous resin; Chinese invention patent (the patent No.: 200710163097.8) disclose a kind of ZANGYINCHEN extract, comprised swertiamarin, gentiopicrin, sweroside, chimonin, 5 kinds of compositions of Lutonaretin; (patent No.: 200910078578.8) disclose a kind of ZANGYINCHEN extract, wherein contained total flavones at least, total flavones accounts for 20 ~ 75% of this ZANGYINCHEN extract to Chinese invention patent; Chinese invention patent (patent No.: 201010176093.5) a kind of method of separating glycoside chemical components in the ZANGYINCHEN is disclosed, comprise extract the ZANGYINCHEN extract aqueous solution, according to polarity gradient extracted component and three processing steps of column chromatographic isolation and purification.But above-mentioned ZANGYINCHEN extraction and separation method only relate to extraction and the ZANGYINCHEN active site resin and the column chromatographic isolation and purification method of ZANGYINCHEN extractum.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of the ZANGYINCHEN effective part extract of a kind of good separating effect, yield height, good product quality.
For addressing the above problem, the preparation method of ZANGYINCHEN effective part extract of the present invention may further comprise the steps:
⑴ by 10 ~ 30 extraordinarily behind pure water or the alcoholic solution merceration 12 ~ 48h of its weight, be supersound extraction 30 ~ 60min under 20 ~ 60 ℃ the condition with dry, as to be cut into 0.5 ~ 2cm segment ZANGYINCHEN raw material in temperature, filter through filter cloth, crude extract;
⑵ after centrifugal remove impurity, obtain centrifugal liquid with described crude extract, and this centrifugal liquid adds pure water to concentrating the front volume amount after concentrating under reduced pressure is removed ethanol, get extracting solution;
⑶ adopt ceramic membrane clarification and the isolating membrance separation mode of ultrafilter membrane to carry out purifies and separates successively described extracting solution, obtains ultra-filtration and separation liquid at last;
⑷ adsorb described ultra-filtration and separation liquid with macroporous resin after, be 20 ~ 60% alcoholic solution eluting, obtain eluent with mass concentration; Described eluent through NF membrane concentrate concentrated solution, this concentrated solution drying promptly gets the ZANGYINCHEN effective part extract to constant weight.
ZANGYINCHEN raw material among the described step ⑴ be meant Swertia mussotii Franch. (
Swertia mussotii), Indian Herba Swertiae bimaculatae (
Swertia chirayita) and Swertia franchetiana H.Smith (
Swertia franchetiana) in a kind of.
The mass concentration of the alcoholic solution among the described step ⑴ is 0 ~ 95%.
Centrifugal rotational speed among the described step ⑵ is 3000 ~ 5000rpm.
Concentrating under reduced pressure condition among the described step ⑵ is meant that vacuum is 0.1 ~ 0.5MPa, and temperature is 50 ~ 80 ℃.
Ceramic membrane membrane aperture among the described step ⑶ is 50nm ~ 800nm.
The organic matter molecular mass of holding back of the ultrafilter membrane among the described step ⑶ is 5000 ~ 50000Dalton.
The organic matter molecular mass of holding back of the NF membrane among the described step ⑷ is 300 ~ 1000Dalton.
Drying among the described step ⑷ is meant a kind of in spray drying, microwave drying or the lyophilization.
Macroporous resin among the described step ⑷ is meant nonpolar or low pole or Semi-polarity macroporous resin.
The present invention compared with prior art has the following advantages:
1, the present invention utilizes ultrasound assisted extraction technique, the ZANGYINCHEN extract that membrane separation technique and resin purification technology make is brown ceramic powder, flavor is extremely bitter, main effective ingredient is gentiopicrin (Gentiopicroside), swertiamarin (Swertiamarin), sweroside (Sweroside), chimonin (Mangiferin), swertianol glycosides (Swertianolin), Lutonaretin (isoorientin), swertisin and and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide (7-O-[α-L-rhamnopyranosyl-(1 → 2)-β-D-xylopyranosyl]-1,8-dihydroxy-3-methoxyxanthone), total content 15.5% ~ 40.4%, wherein gentiopicroside in different morphological 3.4% ~ 20.6%, swertiamarin content 0.6% ~ 4.8%, sweroside content is 0.1% ~ 1.6%, chimonin content 0% ~ 10.6%, swertianol glycosides content 0% ~ 10.2%, Lutonaretin 0% ~ 5.0%, swertisin 0% ~ 8.5%, 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 0% ~ 8.3%.
Temperature was lower when 2, the present invention adopted supersound extraction, and more conventional hot reflux is extracted, and had avoided thermal instability owing to the iridoids material to cause the phenomenon of decomposing, so effective ingredient yield height.
3, the present invention adopts organic membrane and resin combination mode to carry out separation and purification, and separation and purification is effective, active constituent content height, good product quality.
4, the present invention can realize linear amplification, is fit to suitability for industrialized production.
The specific embodiment
Embodiment 1The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Swertia mussotii Franch. raw material 10Kg, be cut into the segment of 0.5 ~ 2cm, after adding 10 times of amount pure water merceration 12 h, the CTXNW-100B combination type circulating ultrasonic extractor of producing with the Beijing Hongxianglong Biotechnology Development Co., Ltd under temperature 20 ℃ (room temperature) extracts 1 time, time 30min, through filter cloth filter crude extract.
⑵ the GQ75 type tube centrifuge that produce crude extract with sky, PVG this centrifugal machine company limited is with the centrifugal 10 ~ 20min of the rotating speed of 3000rpm, and the particulate matter of removing in the crude extract obtains 90Kg centrifugal liquid.
⑶ the SJM-FHM-10 type membrane aperture that adopt the outstanding film engineering of Hefei generation Co., Ltd to produce centrifugal liquid is that the ceramic micro filter film device of 200nm filters, and gets clear liquor 100Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 10Kg).The SJM-DGN-060 type that clear liquor is produced with the outstanding film engineering of Hefei generation Co., Ltd, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 5000Dalton carries out ultrafiltration and holds back separations (process of the test is added the 200Kg pure water), ultra-filtration and separation liquid 280Kg(remains ultrafilter membrane debris 18Kg).
⑷ with ultra-filtration and separation liquid non-polar macroporous resin D101(150*30cm) adsorb after, be 40% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; The SJM-DGN-060 type that eluent is produced through the outstanding film engineering of Hefei generation Co., Ltd, hold back organic matter molecular mass be the NF membrane of 300Dalton concentrate concentrated solution 12Kg, after this concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, the Mini Spray Dryer B-29 type spray dryer that adopts Switzerland BUCHI to produce carries out spray drying, to set tower pathogenic wind-warm degree be 160 ℃, go out the tower pathogenic wind-warm is that 80 ℃, throughput are 20 m/h, be dried to constant weight, promptly get brown ZANGYINCHEN effective part extract 0.2Kg, yield 2.0%.
The Agilent 1200 type high-efficient liquid phase chromatogram HPLCs that this extract is produced through U.S. Agilent company are measured and are contained gentiopicrin 11.6%, swertiamarin 3.4%, sweroside 0.5%, chimonin 0%, swertianol glycosides 0 %, Lutonaretin 0 %, swertisin 0% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 0 % adds up to total content 15.5%.
Embodiment 2The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Swertia mussotii Franch. raw material 5Kg, be cut into the segment of 0.5 ~ 2cm, adding 20 times of amount mass concentrations is behind 30% alcoholic solution merceration 48 h, extracts 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 40 ℃ in temperature, time 30min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 5000rpm crude extract, the particulate matter of removing in the crude extract obtains 96Kg centrifugal liquid, this centrifugal liquid vacuum 0.3MPa and temperature be under 80 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 50nm, gets clear liquor 104Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 9Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 10000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 16Kg of ultra-filtration and separation liquid 288Kg().
⑷ with ultra-filtration and separation liquid non-polar macroporous resin D201(150*30cm) adsorb after, be 20% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 300Dalton concentrate concentrated solution 12Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, adopt FDU-1100 type freezer dryer to carry out lyophilization, chilling temperature is-45 ℃, vacuum is 0.05 ~ 0.1MPa, be dried to constant weight, get brown ZANGYINCHEN effective part extract 0.2Kg, yield 4.0%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 12.6%, swertiamarin 3.5%, sweroside 1.2%, chimonin 3.6%, swertianol glycosides 3.2%, Lutonaretin 2.3 %, swertisin 2.8% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 2.5 % adds up to total content 31.7%.
Embodiment 3The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Swertia franchetiana H.Smith raw material 10Kg, be cut into the segment of 0.5 ~ 2cm, adding 10 times of amount mass concentrations is behind 50% alcoholic solution merceration 24 h, extracts 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 60 ℃ in temperature, time 30min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 4000rpm crude extract, the particulate matter of removing in the crude extract obtains 92Kg centrifugal liquid, this centrifugal liquid vacuum 0.3MPa and temperature be under 70 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 800nm, gets clear liquor 101Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 10Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 50000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 20Kg of ultra-filtration and separation liquid 280Kg().
⑷ with ultra-filtration and separation liquid non-polar macroporous resin HP-20(150*30cm) adsorb after, be 50% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 1000Dalton concentrate concentrated solution 15Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, adopt KMZ-2006 type microwave vacuum dryer to carry out microwave drying, microwave power is 4 ~ 6KW, vacuum is 0.1 ~ 0.5MPa, be dried to constant weight, get brown ZANGYINCHEN effective part extract 0.48Kg, yield 4.8%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 3.4%, swertiamarin 0.6%, sweroside 0.1%, chimonin 1.6%, swertianol glycosides 10.2%, Lutonaretin 3.6 %, swertisin 8.5% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 8.3 % adds up to total content 42.3%.
Embodiment 4The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Indian Herba Swertiae bimaculatae raw material 10Kg, be cut into the segment of 0.5 ~ 2cm, adding 10 times of amount mass concentrations is behind 70% alcoholic solution merceration 36 h, extracts 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 20 ℃ in temperature, time 30min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 3500rpm crude extract, the particulate matter of removing in the crude extract obtains 90Kg centrifugal liquid, this centrifugal liquid vacuum 0.4MPa and temperature be under 70 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 400nm, gets clear liquor 96Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 13Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 10000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 21Kg of ultra-filtration and separation liquid 274Kg().
⑷ with ultra-filtration and separation liquid non-polar macroporous resin XAD-16(150*30cm) adsorb after, be 60% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 500Dalton concentrate concentrated solution 18Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, adopt KMZ-2006 type microwave vacuum dryer to carry out microwave drying, microwave power is 4 ~ 6KW, vacuum is 0.1 ~ 0.5MPa, be dried to constant weight, get brown ZANGYINCHEN effective part extract 0.5Kg, yield 5.0%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 12.8%, swertiamarin 3.2%, sweroside 1.6%, chimonin 9.8%, swertianol glycosides 7.5%, Lutonaretin 0%, swertisin 0% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 0 % adds up to total content 34.9%.
Embodiment 5The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Indian Herba Swertiae bimaculatae raw material 5Kg, be cut into the segment of 0.5 ~ 2cm, adding 20 times of amount mass concentrations is behind 95% alcoholic solution merceration 30 h, extracts 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 40 ℃ in temperature, time 30min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 4500rpm crude extract, the particulate matter of removing in the crude extract obtains 95Kg centrifugal liquid, this centrifugal liquid vacuum 0.1MPa and temperature be under 50 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 50nm, gets clear liquor 102Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 12Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 50000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 18Kg of ultra-filtration and separation liquid 283Kg().
With ultra-filtration and separation liquid with low pole macroporous resin AB-8(150*30cm) adsorb after, be 40% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 300Dalton concentrate concentrated solution 20Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, adopt FDU-1100 type freezer dryer to carry out lyophilization, chilling temperature is-45 ℃, vacuum is 0.05 ~ 0.1MPa, be dried to constant weight, get brown ZANGYINCHEN effective part extract 0.21Kg, yield 4.2%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 11.2%, swertiamarin 3.2%, sweroside 1.5%, chimonin 10.6%, swertianol glycosides 8.6%, Lutonaretin 0%, swertisin 0% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 0 % adds up to total content 35.1%.
Embodiment 6The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Swertia mussotii Franch. raw material 10Kg, be cut into the segment of 0.5 ~ 2cm, after adding 10 times of amounts mass concentrations being 70% alcoholic solution merceration 40h, extract 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 20 ℃ in temperature, time 45min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 4500rpm crude extract, the particulate matter of removing in the crude extract obtains 97Kg centrifugal liquid, this centrifugal liquid vacuum 0.2MPa and temperature be under 60 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 200nm, gets clear liquor 105Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 10Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 50000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 22Kg of ultra-filtration and separation liquid 280Kg().
With ultra-filtration and separation liquid with low pole macroporous resin DM130(150*30cm) adsorb after, be 60% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 500Dalton concentrate concentrated solution 17.5Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, adopt KMZ-2006 type microwave vacuum dryer to carry out microwave drying, microwave power is 4 ~ 6KW, vacuum is 0.1 ~ 0.5MPa, be dried to constant weight, get brown ZANGYINCHEN effective part extract 0.45Kg, yield 4.5%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 8.6%, swertiamarin 2.2%, sweroside 0.8%, chimonin 8.8%, swertianol glycosides 6.3%, Lutonaretin 5.0%, swertisin 4.2% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 4.5% adds up to total content 46.0%.
Embodiment 7The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Indian Herba Swertiae bimaculatae raw material 5Kg, be cut into the segment of 0.5 ~ 2cm, after adding 20 times of amounts mass concentrations being 30% alcoholic solution merceration 30h, extract 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 40 ℃ in temperature, time 60min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 3500rpm crude extract, the particulate matter of removing in the crude extract obtains 92Kg centrifugal liquid, this centrifugal liquid vacuum 0.5MPa and temperature be under 80 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 400nm, gets clear liquor 96Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 12Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 5000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 16Kg of ultra-filtration and separation liquid 275Kg().
With ultra-filtration and separation liquid with Semi-polarity macroporous resin ADS-7(150*30cm) adsorb after, be 20% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 300Dalton concentrate concentrated solution 14Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, adopt FDU-1100 type freezer dryer to carry out lyophilization, chilling temperature is-45 ℃, vacuum is 0.05 ~ 0.1MPa, be dried to constant weight, get brown ZANGYINCHEN effective part extract 0.14Kg, yield 2.8%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 22.6%, swertiamarin 6.8%, sweroside 3.2%, chimonin 0%, swertianol glycosides 0%, Lutonaretin 0%, swertisin 0% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 0 % adds up to total content 27.0%.
Embodiment 8The preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ get exsiccant Swertia franchetiana H.Smith raw material 10Kg, be cut into the segment of 0.5 ~ 2cm, adding 30 times of amount mass concentrations is behind 50% alcoholic solution merceration 24 h, extracts 1 time with CTXNW-100B combination type circulating ultrasonic extractors down for 60 ℃ in temperature, time 30min, through filter cloth filter crude extract.
⑵ use GQ75 type tube centrifuge with the centrifugal 10 ~ 20min remove impurity of the rotating speed of 4000rpm crude extract, the particulate matter of removing in the crude extract obtains 140Kg centrifugal liquid, this centrifugal liquid vacuum 0.2MPa and temperature be under 70 ℃ of conditions after concentrating under reduced pressure is removed ethanol, add pure water to concentrating the front volume amount, get extracting solution.
⑶ adopt SJM-FHM-10 type membrane aperture with extracting solution is the ceramic micro filter film device filtration of 800nm, gets clear liquor 145Kg(process of the test and adds water 20Kg, surplus ceramic membrane filter debris 13Kg).Clear liquor with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 10000Dalton carries out ultrafiltration and holds back separation (process of the test is added the 200Kg pure water), the surplus ultrafilter membrane debris 30Kg of ultra-filtration and separation liquid 405Kg().
With ultra-filtration and separation liquid with Semi-polarity macroporous resin ADS-7(150*30cm) adsorb after, be 50% alcoholic solution eluting with the mass concentration of 6 times of amounts of resin volume (about 300L), obtain eluent; Eluent through the SJM-DGN-060 type, hold back organic matter molecular mass be the NF membrane of 1000Dalton concentrate concentrated solution 20Kg, after the nanofiltration concentrated solution further concentrates with R2002K type 20L Rotary Evaporators, the Mini Spray Dryer B-29 type spray dryer that adopts Switzerland BUCHI to produce carries out spray drying, to set tower pathogenic wind-warm degree be 160 ℃, go out the tower pathogenic wind-warm is that 80 ℃, throughput are 20 m/h, be dried to constant weight, promptly get brown ZANGYINCHEN effective part extract 0.24Kg, yield 4.8%.
This extract is measured through Agilent 1200 type high-efficient liquid phase chromatogram HPLCs and is contained gentiopicrin 2.6%, swertiamarin 0.4%, sweroside 0.1%, chimonin 1.1%, swertianol glycosides 6.0%, Lutonaretin 2.4 %, swertisin 6.5% and 7-O-[α-L-pyrans rhamnose-(1 → 2)-β-D-xylopyranose]-1,8-dihydroxy-3-methoxyl group mouth diphenylene ketone oxide content 7.2 % adds up to total content 34.7%.
Claims (6)
1. the preparation method of ZANGYINCHEN effective part extract may further comprise the steps:
⑴ by 10 ~ 30 extraordinarily behind pure water or the alcoholic solution merceration 12 ~ 48h of its weight, be supersound extraction 30 ~ 60min under 20 ~ 60 ℃ the condition with dry, as to be cut into 0.5 ~ 2cm segment ZANGYINCHEN raw material in temperature, filter through filter cloth, crude extract; Described ZANGYINCHEN raw material is meant a kind of in Swertia mussotii Franch., Indian Herba Swertiae bimaculatae and the Swertia franchetiana H.Smith;
⑵ after centrifugal remove impurity, obtain centrifugal liquid with described crude extract, and this centrifugal liquid adds pure water to concentrating the front volume amount after concentrating under reduced pressure is removed ethanol, get extracting solution;
⑶ adopt ceramic membrane clarification and the isolating membrance separation mode of ultrafilter membrane to carry out purifies and separates successively described extracting solution, obtains ultra-filtration and separation liquid at last; Described ceramic membrane membrane aperture is 50nm ~ 800nm; The organic matter molecular mass of holding back of described ultrafilter membrane is 5000 ~ 50000Dalton;
⑷ adsorb described ultra-filtration and separation liquid with macroporous resin after, be 20 ~ 60% alcoholic solution eluting, obtain eluent with mass concentration; Described eluent through NF membrane concentrate concentrated solution, this concentrated solution drying promptly gets the ZANGYINCHEN effective part extract to constant weight; The organic matter molecular mass of holding back of described NF membrane is 300 ~ 1000Dalton.
2. the preparation method of ZANGYINCHEN effective part extract as claimed in claim 1 is characterized in that: the mass concentration of the alcoholic solution among the described step ⑴ is 0 ~ 95%.
3. the preparation method of ZANGYINCHEN effective part extract as claimed in claim 1 is characterized in that: the centrifugal rotational speed among the described step ⑵ is 3000 ~ 5000rpm.
4. the preparation method of ZANGYINCHEN effective part extract as claimed in claim 1 is characterized in that: the concentrating under reduced pressure condition among the described step ⑵ is meant that vacuum is 0.1 ~ 0.5MPa, and temperature is 50 ~ 80 ℃.
5. the preparation method of ZANGYINCHEN effective part extract as claimed in claim 1 is characterized in that: the drying among the described step ⑷ is meant a kind of in spray drying, microwave drying or the lyophilization.
6. the preparation method of ZANGYINCHEN effective part extract as claimed in claim 1 is characterized in that: the macroporous resin among the described step ⑷ is meant nonpolar or low pole or Semi-polarity macroporous resin.
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CN105434342A (en) * | 2015-12-21 | 2016-03-30 | 贵州瑞和制药有限公司龙里药厂 | Preparation method for Shuganning injection preparation |
CN107375412A (en) * | 2017-08-02 | 2017-11-24 | 色达格萨尔药业有限公司 | The concocting method of mussot swertia herb |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1634099A (en) * | 2003-12-31 | 2005-07-06 | 昆明同持医药研究有限公司 | Swerianmarin injectio, its preparation process and application |
CN101396428A (en) * | 2007-09-30 | 2009-04-01 | 中国科学院西北高原生物研究所 | Tibetan capillary extract and preparation method, medicine composition and use thereof |
CN101935278A (en) * | 2009-06-11 | 2011-01-05 | 周大捷 | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae |
-
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1634099A (en) * | 2003-12-31 | 2005-07-06 | 昆明同持医药研究有限公司 | Swerianmarin injectio, its preparation process and application |
CN101396428A (en) * | 2007-09-30 | 2009-04-01 | 中国科学院西北高原生物研究所 | Tibetan capillary extract and preparation method, medicine composition and use thereof |
CN101935278A (en) * | 2009-06-11 | 2011-01-05 | 周大捷 | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae |
Non-Patent Citations (2)
Title |
---|
9种"藏茵陈"原植物中的7种有效化学成分研究;杨慧玲等;《中草药》;20050831;第36卷(第08期);1233-1237页 * |
杨慧玲等.9种"藏茵陈"原植物中的7种有效化学成分研究.《中草药》.2005,第36卷(第08期),1233-1237页. |
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