CN107213249A - Nine steam the processing procedure method of nine-processing radix rehmanniae preparata - Google Patents

Nine steam the processing procedure method of nine-processing radix rehmanniae preparata Download PDF

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CN107213249A
CN107213249A CN201710282758.2A CN201710282758A CN107213249A CN 107213249 A CN107213249 A CN 107213249A CN 201710282758 A CN201710282758 A CN 201710282758A CN 107213249 A CN107213249 A CN 107213249A
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steam
rehmannia
prepared rhizome
hours
dry
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周青明
茹慈
梁斌
范九良
孙玉
许东亚
郭庆
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Anhui Hua Shan Tang Chinese Herbal Medicine Co Ltd
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Anhui Hua Shan Tang Chinese Herbal Medicine Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/80Scrophulariaceae (Figwort family)
    • A61K36/804Rehmannia
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/13Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting

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Abstract

The invention provides the preferred processing procedure method that nine steam nine-processing radix rehmanniae preparata, by adjusting existing nine technic indexs for steaming just technique processed, so as to optimize the Preparation process of prepared rhizome of rehmannia, drug quality, 5 hydroxymethylfurfurals are favorably improved(HMF)With the content highest of hydroxyethyl methacrylate (HMFA), the drug effect of prepared rhizome of rehmannia is further improved.

Description

Nine steam the processing procedure method of nine-processing radix rehmanniae preparata
Technical field
The present invention relates to the processing work of traditional Chinese medicine processing technique field, more particularly to a kind of nine steaming nine-processing radix rehmanniae preparatas of optimization Process.
Background technology
Glutinous rehmannia is scrophulariaceae rehmannia glutinosa plantRehmannia glutinosa Libosch.Root tuber.First recorded in《Legendary god of farming's sheet Grass warp》, it is classified as top grade.History tree is on the books, is one of conventional Chinese medicine.Glutinous rehmannia, which is used as medicine, to be divided into:It is fresh rehmannia root, dried rehamnnia root, ripe Glutinous rehmannia, radix rehmanniae recen charcoal, prepared rhizome of rehmannia charcoal etc..Glutinous rehmannia is after different concocting method processing, and its nature and flavor, effect also occur accordingly Change.Fresh rehmannia root is cold in nature, sweet-bitter flavor, based on clearing heat and promoting fluid, cooling blood and hemostasis.Fresh rehmannia root is processed to dry rear name dried rehamnnia root or life Glutinous rehmannia, its is cold in nature, sweet, based on clearing heat and cooling blood, nourishing Yin and promoting production of body fluid.Dried rehamnnia root name prepared rhizome of rehmannia after steaming, its property turns temperature by cold, Its taste turns sweet by hardship, and its effect is turned to mend by clear, with nourishing yin and supplementing blood, based on beneficial to spirit and marrow.Clinic is according to its different effect, difference For different diseases.The concocting method of glutinous rehmannia and the quality of processed product can directly produce influence to clinical efficacy.Make a general survey of the successive dynasties Book on Chinese herbal medicine, the concocting method of glutinous rehmannia has as many as more than ten kinds, and some methods are used till today.But many concocting methods do not find it is optimal The condition of change, has influence on clinical accurate medication.
Glutinous rehmannia is recorded using Powder Made by Steamed Method processing earliest documents and sees Han dynasty《Synopsis of Prescriptions of the Golden Chamber》:"  nozzles, steaming as bucket rice Meal long, its juice is contained with bronze, brass or copper ware, more twists glutinous rehmannia juice ".In the Southern Qi Dynasty《Liu Juanzi Guiyi Fang, Liu Juanzi》In have:" cutting, steam roasting ", Tang《Medical secrets of official》 Have:The record of " frittering the extremely ripe of steaming ".The word of prepared rhizome of rehmannia one is first appeared in Tang's SUN Si miao《Essential Recipes for Emergent Use Worth A Thousand Gold》, its concocting method is " fief Huang, removes its palpus, leaf and radicula, smashes strand juice with stain fertilizer person, writes in rice steamer, if native rice is without to cover, steaming a period of time goes out, cruelly It is dry, in interior juice, and steamed juice, go out to the greatest extent, just the universe it." SUN Si miao《Qianjin Yi Fang》Say:" jin number is picked to select and thought of a way surely, is soaked settled, is waited It is good fine day just early to steam it, i.e., it is sudden and violent in day, night put in juice with thing lid it, the Ming Dynasty steams again, and Gu Fajiu the present but sees that the most color of juice is black all over stopping It is ripe, steam three, five times also ".The requirement of its concocting process steams three again, five times, quality requirement color is black." Gu Fajiu times described in text Only " understand, processing prepared rhizome of rehmannia steams multiple method to be had before this, but there is not yet document is recorded.Song Dynasty is to prepared rhizome of rehmannia The standard of steaming proposes further requirement,《Classified Materia Meidca》Draw figure through saying " the method that the present does:Take fertile glutinous rehmannia three, 20 jin, wash Only, more to pick radicula and the thin short person of root section, also two, 30 jins, smash strand and take juice, throw in silver-bearing copper device, lower fertile glutinous rehmannia leaching is filtered meeting Soak through, three, four mistakes are steamed on meal, constantly leaching, which is filtered, turns, and steams settled and sudden and violent, making juice, gold-tinted is black as painted with using up it, sweet such as maltose ".To cultivated land The quality of yellow processed product proposes the quality standard of " light is black as painted, sweet such as maltosemalt sugar ".This quality criteria requirements one of prepared rhizome of rehmannia Directly use till today.
Successive dynasties process prepared rhizome of rehmannia with wine and use yellow rice wine, and are preferred with Shaoxing production yellow rice wine, it is believed that:Prepared rhizome of rehmannia matter savoury is dense, Grow it is greasy hinder after stomach, wine then property turn temperature master and enrich blood, and capacity for liquor row can be borrowed to dissipate, play row medicine gesture, the effect of promoting blood circulation is more favourable to mend Blood, make glutinous rehmannia mend and it is oiliness.The dried rhizome of rehmannia is different from cultivated land pharmacological action, and the dried rhizome of rehmannia is cold in nature, and function is heat clearing and blood cooling, enriching yin benefit Kidney, promote the production of body fluid to quench thirst, be usually used in the diseases such as treatment steaming bone and consumptive fever, throat pain, blood-stained sputum.The dried rhizome of rehmannia is made after cultivated land, and the property of medicine is by trembling with fear Become tepor, its function also changes, as antianaemics.The method document that prepared rhizome of rehmannia is processed is recorded and is not quite similar, have " steaming three, Five times ", " nine steam nine make " etc., but rule of thumb process mostly, can not still find optimal concocting method, these are to prepared rhizome of rehmannia big gun Though the quality requirement of product, which is attained by the standard of " light is black as painted, sweet such as maltosemalt sugar ", drug effect, lacks difference, direct shadow Ring the curative effect of curing the disease to prepared rhizome of rehmannia processed product.Ancients have found that only nine steam the cultivated land of nine systems, could fully go by clinical practice Its is cold, is changed into warm medicine, and effect of its kidney-replenishing blood-nourishing can just be embodied, therefore, and three, steam for five times and can not reach drug effect.
In the processing procedure of prepared rhizome of rehmannia, although the conventional system of nine steaming nine reaches requirement in appearance luster, due to its work Skill is complicated, and condition is various, and cost is high, and processing procedure process is based on the experience of clinical medicine work, random big, is easiest to occur The not good situation of effect is processed, the increase of its active ingredient, the reduction of toxic component can not be optimal, and therefore, not be A kind of processing procedure of main flow, but also just because of this fine concocting method, once condition is suitable, the prepared rhizome of rehmannia processed out Drug effect is extremely effective.
Generally it is the standard of consistent i.e. " light is black as painted, sweet such as maltosemalt sugar " to the quality requirement of prepared rhizome of rehmannia processed product, and it is every There is the finished product after larger difference, therefore prepared slices of Chinese crude drugs processing in the colour vision of individual, the sense of taste, its quality is uneven.
The present invention is optimized in the processing procedure that nine systems are steamed to nine, finds out optimal processing condition, and by more Specific parameter index carries out quality verification to processing product, obtains optimal processing procedure.
The content of the invention
It is that the processing of the clinical medicine adds the invention provides the concocting method and quality control standard that nine steam nine-processing radix rehmanniae preparata Work provides specification foundation, by new concocting method and process conditions, is favorably improved drug quality, 5 hydroxymethyl furfural(HMF) With the content highest of hydroxyethyl methacrylate (HMFA), the drug effect of prepared rhizome of rehmannia is further improved.
Based on this, the present invention provides a kind of nine nine concocting methods processed of steaming of prepared rhizome of rehmannia, and it includes:
The first step, selection;
Second step, wash;
3rd step, one, which steams one, makes;
4th step, two, which steam two, makes;
5th step, three, which steam three, makes;
6th step, four, which steam four, makes;
7th step, five, which steam five, makes;
8th step, six, which steam six, makes;
9th step, seven, which steam seven, makes;
Tenth step, eight, which steam eight, makes;
11st step, nine, which steam nine, makes;
12nd step, sterilizing, packaging;
Wherein, the nine steaming temperature scopes for steaming nine-processing radix rehmanniae preparata are 130 DEG C~150 DEG C in the concocting method.
Wherein, nine pressure limits for steaming nine-processing radix rehmanniae preparata are 0.2Mpa~0.4Mpa in the concocting method.
Wherein, the mass ratio of radix rehmanniae recen to be processed used in nine steaming nine-processing radix rehmanniae preparatas in the concocting method and yellow rice wine Example is 3:1~2:1.
Wherein, the 3rd step is specially further:
A is walked, and the radix rehmanniae recen after net system is placed in Turnround basket by infusing drugs in wine, plus yellow rice wine, and yellow rice wine amount is the 20% of total yellow rice wine addition ~25% is advisable, and infiltration is sucked for 2~4 hours to wine, and half an hour is stirred once;
B is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, middle product are put into tilting-type digester or uniformly inserted in food steamer, the steaming that pressure is 0.2~0.4Mpa is passed through Vapour stops steam one night of vexed profit for about 8 hours, and steaming temperature scope is 130 DEG C~150 DEG C, steams to inside and outside in moist black, in pouring out Liquid and prepared rhizome of rehmannia that face is steamed;
C is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
D is walked, and is mixed, and mixes first time distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary, obtain middle product.
Wherein, the 4th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 6 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes second of distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
Wherein, the 5th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes third time distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
11st step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to six, seventy percent it is dry or spread out and dried in the air naturally system in field processed It is dry to six, seventy percent;
C is walked, and is dried, and is performed《Dry post standard practice instructions》,《Heated-air circulation oven standard practice instructions》Or《Opened type Baking oven standard practice instructions》, 55~60 DEG C of design temperature, thickness:25~30mm, about 36 hours time, dried moisture control System is within 15.0 ﹪.
The present invention also provides the prepared rhizome of rehmannia prepared using the above method.
HMF detects that peak area preferably 3500000~3700000, HMFA detects peak through HPLC through HPLC in the prepared rhizome of rehmannia Area preferably 280000~300000.
Beneficial technique effect
The present invention by test obtain nine steam nine-processing radix rehmanniae preparatas optimal processing conditions, be favorably improved drug quality and drug effect into Point, 5 hydroxymethyl furfural(HMF)With the content highest of hydroxyethyl methacrylate (HMFA), the medicine of prepared rhizome of rehmannia is further improved Effect.
Embodiment
In the preparation technology for processing prepared rhizome of rehmannia, temperature, pressure, the consumption of yellow rice wine are three topmost condition elements, are led to Cross substantial amounts of orthogonal test of the invention to draw, temperature is the most important factor that influence processes prepared rhizome of rehmannia drug effect quality, to be obtained Nine steam nine-processing radix rehmanniae preparata Optimal Temperature scope for 130 DEG C~150 DEG C, and optimal temperature is 140 DEG C, pressure 0.2Mpa~0.4Mpa Properly, optimum pressure is 0.3Mpa, radix rehmanniae recen and yellow rice wine usage ratio 3:1~2:1 is suitable, and we select 2:1 is best proportion. We analyze this optimal preparation condition, if temperature is less than 130 DEG C, cultivated land is not easy to be steamed, and the time steamed can prolong Long, control of microorganisms is poor in addition, if temperature is higher than 150 DEG C, cultivated land is easily steaming process China and foreign countries Jiao Lisheng, and influence is effective Composition;If pressure is less than 0.2Mpa, yellow rice wine is not easy to steam into cultivated land, if pressure is more than 0.4Mpa, it is higher to equipment requirement and Energy resource consumption is excessive, not economical and practical enough;If the ratio of glutinous rehmannia and yellow rice wine is more than 3:1, then the amount of yellow rice wine is not enough, it is impossible to steam completely Saturating glutinous rehmannia, if the ratio of glutinous rehmannia and yellow rice wine is less than 2:1, then the amount of yellow rice wine is excessive, the overlong time steamed, the consumption of yellow rice wine It is many, it is not economical and practical enough, and one steam one it is processed when, use yellow rice wine amount more, could soak saturating, preferably take up whole yellow rice wine consumption 20%~25%, be easy to steam acquisition active ingredient as much as possible for the first time, steam for the last time used in yellow rice wine amount It is more, occupy the 20%~25% of whole yellow rice wine consumption.
Yellow rice wine preferably selects the strong yellow wine of more than 5 years, and the property of its diverging weakens, and the property of temperature compensation strengthens, therefore chooses old Huang Wine steams glutinous rehmannia, makes the temperature compensation drug effect of prepared rhizome of rehmannia stronger, and the strong yellow wine of more than 5 years of Shaoxing production is selected in the present invention, and such as Fruit yellow rice wine is then unable to reach this effect, the temperature compensation performance of prepared rhizome of rehmannia is very weak from the wine product newly dispatched from the factory.
The processing procedure method for the prepared rhizome of rehmannia that the present invention is provided is specifically included:
The first step, chooses, and performs《Clean post standard practice instructions》, impurity is sorted out from radix rehmanniae recen, clean transfer container is put In, weigh, section, thickness is in 25~30mm;
Second step, wash is performed《Wash post standard practice instructions》And《Medicine-washing machine standard practice instructions》, wash post behaviour Prepared rhizome of rehmannia is put into machine by workmanship, with meet the water washing 3 times of drinking water standard to it is clean, without silt, load clean plastics week Turn container;
3rd step, one, which steams one, makes;
4th step, two, which steam two, makes;
5th step, three, which steam three, makes;
6th step, four, which steam four, makes;
7th step, five, which steam five, makes;
8th step, six, which steam six, makes;
9th step, seven, which steam seven, makes;
Tenth step, eight, which steam eight, makes;
11st step, nine, which steam nine, makes;
12nd step, sterilizing is packed with packaging directive, is performed《Pack post standard practice instructions》, it is desirable to it is accurate to weigh, sealing Tightly, no folder medicine, leakage medicine phenomenon, often pack and post the quality certification, quality certification content complete display.
3rd step is specially further:
A is walked, and the radix rehmanniae recen after net system is placed in Turnround basket by infusing drugs in wine, plus yellow rice wine, and yellow rice wine amount is the 20% of total yellow rice wine addition ~25% is advisable, and infiltration is sucked for 2~4 hours to wine, and half an hour is stirred once;
B is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, middle product are put into tilting-type digester or uniformly inserted in food steamer, the steaming that pressure is 0.2~0.4Mpa is passed through Vapour stops steam one night of vexed profit for about 8 hours, and steaming temperature scope is 130 DEG C~150 DEG C, steams to inside and outside in moist black, in pouring out Liquid and prepared rhizome of rehmannia that face is steamed;
C is walked, and prepared rhizome of rehmannia is dried:Temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
D is walked, and is mixed, and mixes first time distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary, obtain middle product.
4th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 6 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes second of distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
5th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
Mix:Mix third time distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour is stirred once.
6th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes the 4th distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
7th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes the 5th distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
8th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes the 6th distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
9th step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes the 7th distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
Tenth step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, steaming temperature scope is 130 DEG C~150 DEG C, stops the vexed profit of steam 2 hours, pours out what the inside was steamed Liquid and prepared rhizome of rehmannia;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes the 7th distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
11st step is specially further:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, middle product are put into tilting-type digester or uniformly inserted in food steamer, yellow rice wine is supplemented, yellow rice wine magnitude of recruitment is total yellow The 20%~25% of wine addition is advisable, and is passed through the steam about 4 hours that pressure is 0.2~0.4Mpa, and steaming temperature scope is 130 DEG C ~150 DEG C, stop the vexed profit of steam 2 hours, pour out the liquid that steams of the inside and prepared rhizome of rehmannia is mixed thoroughly;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to six, seventy percent it is dry or spread out and dried in the air naturally system in field processed It is dry to six, seventy percent;
C is walked, and is dried, and is performed《Dry post standard practice instructions》,《Heated-air circulation oven standard practice instructions》Or《Opened type Baking oven standard practice instructions》, 55~60 DEG C of design temperature, product prepared rhizome of rehmannia 25~30mm of thickness, about 36 hours time, after drying Moisture control within 15.0 ﹪.
Describe embodiments of the present invention in detail using embodiment below, whereby to the present invention how application technology means To solve technical problem, and reach the implementation process of technique effect and can fully understand and implement according to this.
Embodiment nine steams nine-processing radix rehmanniae preparata
Process medicine:Radix rehmanniae recen medicine materical crude slice
Yellow rice wine preferably selects the strong yellow wine of more than 5 years, and the property of its diverging weakens, and the property of temperature compensation strengthens, therefore chooses old yellow rice wine and steam Prepared glutinous rehmannia, makes the temperature compensation drug effect of prepared rhizome of rehmannia stronger, and the strong yellow wine of more than 5 years of Shaoxing production is selected in the present invention, and if yellow Wine is then unable to reach this effect, the temperature compensation performance of prepared rhizome of rehmannia is very weak from the wine product newly dispatched from the factory.
600g radix rehmanniae recens are chosen, are performed《Clean post standard practice instructions》, impurity is sorted out from radix rehmanniae recen, clean week is put Turn in container, weigh, section, thickness is between 25~30mm.
Perform《Wash post standard practice instructions》And《Medicine-washing machine standard practice instructions》, wash post operation work will be ripe Glutinous rehmannia is put into machine, with meet the water washing 3 times of drinking water standard to it is clean, without silt, load clean plastics transfer container.
One, which steams one, makes:By 60kg radix rehmanniae recen infusings drugs in wine, the radix rehmanniae recen after net system is placed in Turnround basket, plus yellow rice wine, yellow rice wine amount For 8kg, infiltration is sucked for 4 hours to wine, and half an hour is stirred once;Steam, perform《Steam post standard practice instructions》And《Steam Saucepan standard practice instructions》Or《Food steamer standard practice instructions》, middle product are put into tilting-type digester or uniformly steaming are inserted In cage, it is passed through the steam that pressure is 0.4Mpa and stops within 8 hours steam one night of vexed profit, steaming temperature scope is 140 DEG C, steaming is in inside and outside Black is moistened, liquid and prepared rhizome of rehmannia that the inside is steamed is poured out;Under the conditions of temperature is 60 DEG C, prepared rhizome of rehmannia about 36 hours to eight is dried Made naturally near dry in field processed into doing or spreading out, mix first time distillate and dried prepared rhizome of rehmannia thoroughly infiltration 4 hours, half an hour Stir once, obtain middle product.
Two, which steam two, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, one is steamed in the middle product input tilting-type digester that a system is obtained or is uniformly inserted in food steamer, plus yellow rice wine 2kg, is passed through the steam 6 hours that pressure is 0.3Mpa, and steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the inside The liquid and prepared rhizome of rehmannia steamed;Prepared rhizome of rehmannia is dried, and temperature is 60 DEG C, dry 36 hours to eighty per cant it is dry or spread out and made naturally extremely in field processed It is near dry;Mix second of distillate and dried prepared rhizome of rehmannia thoroughly infiltration 4 hours, half an hour is stirred once.
Three, which steam three, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, plus yellow rice wine 2kg, being passed through pressure is 0.3Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the liquid that steams of the inside and ripe Glutinous rehmannia;Prepared rhizome of rehmannia dry, temperature be 60 DEG C, dry 36 hours to eighty per cant it is dry or spread out in field processed make naturally to closely do;Will third time Distillate mixes infiltration 4 hours thoroughly with dried prepared rhizome of rehmannia, and half an hour is stirred once.
Four, which steam four, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, plus yellow rice wine 2kg, being passed through pressure is 0.3Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the liquid that steams of the inside and ripe Glutinous rehmannia;Prepared rhizome of rehmannia dry, temperature be 60 DEG C, dry 36 hours to eighty per cant it is dry or spread out in field processed make naturally to closely do;By the 4th time Distillate mixes infiltration 4 hours thoroughly with dried prepared rhizome of rehmannia, and half an hour is stirred once.
Five, which steam five, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, plus yellow rice wine 2kg, being passed through pressure is 0.3Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the liquid that steams of the inside and ripe Glutinous rehmannia;Prepared rhizome of rehmannia dry, temperature be 60 DEG C, dry 36 hours to eighty per cant it is dry or spread out in field processed make naturally to closely do;By the 5th time Distillate mixes infiltration 4 hours thoroughly with dried prepared rhizome of rehmannia, and half an hour is stirred once.
Six, which steam six, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, plus yellow rice wine 2kg, being passed through pressure is 0.3Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the liquid that steams of the inside and ripe Glutinous rehmannia;Prepared rhizome of rehmannia dry, temperature be 60 DEG C, dry 36 hours to eighty per cant it is dry or spread out in field processed make naturally to closely do;By the 6th time Distillate mixes infiltration 4 hours thoroughly with dried prepared rhizome of rehmannia, and half an hour is stirred once.
Seven, which steam seven, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, plus yellow rice wine 2kg, being passed through pressure is 0.3Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the liquid that steams of the inside and ripe Glutinous rehmannia;Prepared rhizome of rehmannia dry, temperature be 60 DEG C, dry 36 hours to eighty per cant it is dry or spread out in field processed make naturally to closely do;By the 7th time Distillate mixes infiltration 4 hours thoroughly with dried prepared rhizome of rehmannia, and half an hour is stirred once.
Eight, which steam eight, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, plus yellow rice wine 2kg, being passed through pressure is 0.3Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pours out the liquid that steams of the inside and ripe Glutinous rehmannia;Prepared rhizome of rehmannia dry, temperature be 60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out in field processed make naturally to closely do;By the 7th Secondary distillate mixes infiltration 4 hours thoroughly with dried prepared rhizome of rehmannia, and half an hour is stirred once.
Nine, which steam nine, makes:Steam, perform《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer Standard practice instructions》, middle product are put into tilting-type digester or uniformly inserted in food steamer, yellow rice wine 8kg is supplemented, is passed through pressure For 0.4Mpa steam 4 hours, steaming temperature scope is 140 DEG C, stops the vexed profit of steam 2 hours, pour out liquid that the inside steams and Prepared rhizome of rehmannia is mixed thoroughly;Prepared rhizome of rehmannia is dried, and temperature is 60 DEG C, dry 36 hours to six, seventy percent it is dry or spread out dried in the air naturally in field processed make to six, Seventy percent is dry;Prepared rhizome of rehmannia is dried again, is performed《Dry post standard practice instructions》,《Heated-air circulation oven standard practice instructions》Or 《Opened type baking oven standard practice instructions》, 60 DEG C of design temperature, thickness:25~30mm, about 36 hours time, dried moisture Control is within 15.0 ﹪.
Test the comparison that one or nine nine cultivated lands processed of steaming steam three cultivated land active ingredients processed with commercially available radix rehmanniae recen, three
Medicinal material:The nine nine cultivated land embodiments 1 processed of steaming that Chinese medicine preparation method of the present invention is processed, numbering is 1.
Commercially available radix rehmanniae recen, prepared rhizome of rehmannia are purchased from the market(Three, which steam three, makes)And nine steam nine-processing radix rehmanniae preparata (condition is unknown), Numbering is 2 respectively:Radix rehmanniae recen, 3:Prepared rhizome of rehmannia, 4:Nine steam nine-processing radix rehmanniae preparata, purchased from large-scale pharmacy of Hefei City, every kind of medicinal material purchase 3 batches are put, all medicinal materials, through Anguo City Chinese medicine row expert appraisal, are certified products.
Laboratory apparatus:P3000 high performance liquid chromatographs;Welchrom C18 chromatographic columns(4.6mm × 250mm, 5 μm); AG204 electronic analytical balances;RE~52A Rotary Evaporators(Shanghai Yarong Biochemical Instrument Plant);The micro high speed centrifugations of TG16~W Machine;The thermostatic water-circulator bath of HH~601.
Experiment reagent:5 hydroxymethyl furfural(HMF)With 5-HMFA (HMFA) reference substance(Two kinds of materials are prepared rhizome of rehmannia Identification material, with standard items draw standard curve)There is provided, determined through HPLC without miscellaneous for preclinical medicine institute of Anhui University of Chinese Medecine Peak, meets qualitative requirement.
Sample preparation methods:Dried all kinds of glutinous rehmannia are prepared into coarse powder with powder beater respectively, granularity can all pass through Particle diameter is No. two sieves of 24 mesh, and precision weighs each medicinal powder 1.0g, put in round-bottomed flask, and accurate addition methanol 50mL is weighed heavy Amount, heating and refluxing extraction 1.5h lets cool, the weight of less loss is supplied with methanol, is shaken up, and filters, and precision measures subsequent filtrate 25mL, Concentrated by rotary evaporation is transferred in 5mL measuring bottles, constant volume shakes up, through 0.45 μ near dry, the residue methanol of volume fraction 15% dissolving M membrane filtrations, it is standby.
Chromatographic condition:WelcHrom C18 chromatographic columns(4.6 mm × 250 mm, 5 μm), the mL/min of flow velocity 1.0, inspection Survey wavelength is 284nm, 35 DEG C of column temperature, the μ L of sample size 20.Binary gradient elutes, mobile phase A is acetonitrile, and B is volume fraction 0.1% phosphate aqueous solution(Elution program:0 ~ 5min, 1%A;5 ~ 10min, 1% ~ 4%A;10 ~ 22min, 4% ~ 6%A;22 ~ 30min, 6% ~ 18%A;30 ~ 60min, 18% ~ 25%A;60 ~ 80min, 25% ~ 35%A).
Precision:Experiment carries out HPLC analyses, continuous sample introduction 5 times, record to same sample solution by foregoing chromatographic condition Retention time and each peak peak area.
Repeated experiment:Same 5 parts of medicinal material is taken, is operated by aforementioned preparation process, prepares sample solution, by foregoing chromatostrip Part carries out HPLC analyses, record retention time and each peak peak area.
Stability:Test same sample solution, room temperature storage, respectively at 0,4,8,12,24,48h, by foregoing chromatographic condition Carry out HPLC analyses, record retention time and each peak peak area.
Product prepared rhizome of rehmannia Characters Identification standard:Irregular sheet or block, surface corvinus is glossy, and stickiness is big, and matter is soft It is soft and with toughness, be not easily broken, section corvinus, glossy, gas is micro-, taste sweet tea.
As a result
Quality control standard of the present invention processes glutinous rehmannia and contrasted with commercially available Characters of Rehmannia glutinosa Libosch. Varieties
Quality control standard of the present invention processes glutinous rehmannia compared with commercially available radix rehmanniae recen, there is larger difference in character, and the present invention is processed Glutinous rehmannia " the black such as paint of color, sweet such as maltosemalt sugar ", soft texture, simultaneous with wilfulness, solid colour in table, is corvinus after incision.City Radix rehmanniae recen is sold in dark-brown, quality is harder, and toughness is relatively strong, after incision, in shallow in table depth.Three steam three cultivated land yellow colors depths processed Brown, quality is relatively soft, and preferably, color is relatively deep in table after incision, is black, but glossiness is uneven for toughness.Commercially available nine Steam nine-processing radix rehmanniae preparata appearance color pitch-black, preferably, color is more consistent in table after incision for glossiness, viscosity processes ripe with the present invention Ground compares, relatively poor, awaits further identification and processes glutinous rehmannia difference with the present invention.
The foundation and optimization of chromatographic condition
284nm is HMF and HMFA Detection wavelength, and it is one of most significant composition of change before and after glutinous rehmannia processes.Therefore, this reality Test with reference to version in 2015《Chinese Pharmacopoeia》Raw, the assay chromatographic condition of prepared rhizome of rehmannia, and eluent gradient program is carried out excellent Change, to obtain as far as possible many shared peak information, the chromatographic condition finally determined.Analyzed using multiple wavelength, sample room can The shared peak increase of identification, the difference that can more accurately reflect between medicinal material.
Method validation
In precision, repeatability and stability experiment, the RSD for measuring its shared peak relative retention time and relative peak area is equal Within 1.1% and 4.7%, show that the precision and method repeatability of instrument are good, sample is stable in 48h at room temperature.
The preparation result of the HMF reference substance standard curves of table 1
Sequence number 1 2 3 4 5 6 7
Sample size μ g 0.0506 0.1518 0.3036 0.6072 1.2144 1.8216 2.4288
Peak area 354548 1154975 2305415 4615483 9249845 13918445 18564842
The preparation result of the HMFA reference substance standard curves of table 2
Sequence number 1 2 3 4 5 6 7
Sample size μ g 0.0113 0.0339 0.1017 0.1526 0.2034 0.3051 0.4068
Peak area 354548 1154975 2305415 4615483 9249845 13918445 18564842
Prepared rhizome of rehmannia sample is determined
Prepared rhizome of rehmannia sample solution is taken, HPLC analyses is carried out by foregoing chromatographic condition, is drawn with HMF and HMFA standard items HPLC Standard curve is reference.
Different sample HMF, HMFA the absworption peak area results of table 3
Sample HMF peak area/105 HMFA peak area/105
Radix rehmanniae recen 679554* 364841*
Commercially available prepared rhizome of rehmannia(Three, which steam three, makes) 1135484* 334541*
Commercially available prepared rhizome of rehmannia(Nine, which steam nine, makes) 2648479* 304879
The present invention processes prepared rhizome of rehmannia 3654814 289747
Prepared rhizome of rehmannia is processed with the present invention to be compared,*P<0.05。
All data are with sample of the same race, and three batch the data obtained averages are defined.
The height of HMF and HMFA growing amounts directly affects the performance of prescription subjective role.Studies have reported that, HMF and Although HMFA medicinal materials contain in itself, relative amount is relatively low, and its main accumulation is largely given birth in glutinous rehmannia concocting process Into, therefore the content that method for processing rehmannia root directly affects two compositions is accumulated, it is heated that the HMF in prepared rhizome of rehmannia mostlys come from processing The dehydration conversion of monose in journey, heat time and temperature have a major impact to its yield, and monose is continuous in the short period of time Dehydration conversion, show as HMF increases with the extension of heat time.Research finds that HMF has certain pharmacological activity, such as drop blood Sugar, improve learning and memory, the effect of resisting myocardial ischemia etc., the pharmacological component of prepared rhizome of rehmannia effect.And HMFA be by HMF oxidation and Come, control HMF degree of oxidations, had a very important role for retaining active ingredient.Therefore, of a relatively high HMF production Raw and relatively low HMFA generation, is the quality control requirement of prepared rhizome of rehmannia more Chinese medicine.
In summary, research shows, the HMF and HMFA of in the market prepared rhizome of rehmannia commodity content can not reach prepared rhizome of rehmannia Quality standard.This experiment is quantified using HPLC methods to HMF and HMFA contained by present invention processing prepared rhizome of rehmannia On the basis of analysis, its quantitative change rule in different concocting process is illustrated, the real scientific meaning of glutinous rehmannia processing is disclosed.
By previous experiments it can be seen that, although be all the system of nine steaming nine, but obtain prepared rhizome of rehmannia HMF and HMFA contents And differ, therefore, the prepared rhizome of rehmannia quality to be optimal, it is necessary to which the preparation condition that nine systems are steamed to nine is groped, this Shen It please pass through substantial amounts of orthogonal experiment, it is the most important factor for prepared rhizome of rehmannia HMF, HMFA amount that influence is processed to find temperature, to obtain Optimal processing condition is obtained, the experimental verification of optimal conditions is carried out below.
Test the comparison of the different preparation condition active ingredients of the cultivated land processed of two or nine steaming nine
Medicinal material:Nine nine cultivated lands processed of steaming that Chinese medicine preparation method of the present invention is processed, using temperature as the principal element for research of starting with, with whole Nine nine systems of steaming that individual concocting process temperature is nine nine cultivated lands processed of steaming of 100 DEG C of processings, whole concocting process temperature is 140 DEG C of processings Cultivated land, whole concocting process temperature are that nine nine cultivated lands processed of steaming of 180 DEG C of processings are research material, and numbering is 1,2,3 respectively.
Laboratory apparatus:P3000 high performance liquid chromatographs;Welchrom C18 chromatographic columns(4.6mm × 250mm, 5 μm); AG204 electronic analytical balances;RE~52A Rotary Evaporators(Shanghai Yarong Biochemical Instrument Plant);The micro high speed centrifugations of TG16~W Machine;The thermostatic water-circulator bath of HH~601.
Experiment reagent:5 hydroxymethyl furfural(HMF)With 5-HMFA (HMFA) reference substance(Two kinds of materials are prepared rhizome of rehmannia Material is identified, standard curve is drawn with standard items)There is provided, determined through HPLC without miscellaneous for preclinical medicine institute of Anhui University of Chinese Medecine Peak, meets qualitative requirement.
Sample preparation methods:Dried all kinds of glutinous rehmannia are prepared into coarse powder with powder beater respectively, granularity can all pass through No. two sieves of 24 purpose of particle diameter, precision weighs each medicinal powder 1.0g, put in round-bottomed flask, accurate addition methanol 50mL, weighed heavy Amount, heating and refluxing extraction 1.5h lets cool, the weight of less loss is supplied with methanol, is shaken up, and filters, and precision measures subsequent filtrate 25mL, Concentrated by rotary evaporation is transferred in 5mL measuring bottles, constant volume shakes up, through 0.45 μ near dry, the residue methanol of volume fraction 15% dissolving M membrane filtrations, it is standby.
Chromatographic condition:WelcHrom C18 chromatographic columns(4.6 mm × 250 mm, 5 μm), the mL/min of flow velocity 1.0, inspection Survey wavelength is 284nm, 35 DEG C of column temperature, the μ L of sample size 20.Binary gradient elutes, mobile phase A is acetonitrile, and B is volume fraction 0.1% phosphate aqueous solution(Elution program:0 ~ 5min, 1%A;5 ~ 10min, 1% ~ 4%A;10 ~ 22min, 4% ~ 6%A;22 ~ 30min, 6% ~ 18%A;30 ~ 60min, 18% ~ 25%A;60 ~ 80min, 25% ~ 35%A).
Precision:Experiment carries out HPLC analyses, continuous sample introduction 5 times, record to same sample solution by foregoing chromatographic condition Retention time and each peak peak area.
Repeated experiment:Same 5 parts of medicinal material is taken, is operated by aforementioned preparation process, prepares sample solution, by foregoing chromatostrip Part carries out HPLC analyses, record retention time and each peak peak area.
Stability:Test same sample solution, room temperature storage, respectively at 0,4,8,12,24,48h, by foregoing chromatographic condition Carry out HPLC analyses, record retention time and each peak peak area.
As a result
Prepared rhizome of rehmannia character pair ratio obtained by three groups of preparation technologies
1st, 2 groups of cultivated lands are met " the black such as paint of color, sweet such as maltosemalt sugar ", soft texture, simultaneous with wilfulness, color one in table after incision Cause, be corvinus, although and 3 groups of cultivated lands also relatively meet standard in appearance, be charred smell, the possible adherent cultivated land in part because Heating-up temperature is too high, occurs processing excessive situation, how is its effect, awaits further identification.
The foundation and optimization of chromatographic condition
284nm is HMF Detection wavelength, and it is one of most significant composition of change before and after glutinous rehmannia processes.Therefore, this laboratory reference Version in 2015《Chinese Pharmacopoeia》Raw, the assay chromatographic condition of prepared rhizome of rehmannia, and eluent gradient program is optimized, to obtain Must be tried one's best many shared peak information, the chromatographic condition finally determined.Analyzed using multiple wavelength, sample room is recognizable to be total to There is peak increase, the difference that can more accurately reflect between medicinal material.
Method validation
In precision, repeatability and stability experiment, the RSD for measuring its shared peak relative retention time and relative peak area is equal Within 1.1% and 4.7%, show that the precision and method repeatability of instrument are good, sample is stable in 48h at room temperature.
Prepared rhizome of rehmannia sample is determined
Prepared rhizome of rehmannia sample solution is taken, HPLC analyses is carried out by foregoing chromatographic condition, is drawn with HMF and HMFA standard items HPLC Standard curve is refers to, and HMF and HMFA standard curve are shown in Tables 1 and 2.
Different sample HMF, HMFA the absworption peak area results of table 4
Sample HMF peak area/105 HMFA peak area/105
①100℃ 3015148* 332448*
②140℃(It is optimal) 3648461 290154
③180℃ 1578116* 395487*
Prepared rhizome of rehmannia is processed with 140 DEG C to be compared,*P<0.05
All data are with sample of the same race, and three batch the data obtained averages are defined.
Optimum process cultivated land sample HMF, HMFA absworption peak area results twice of table 5
Sample HMF peak area/105 HMFA peak area/105
Test a prepared rhizome of rehmannia 3654814 289747
Test two prepared rhizomes of rehmannia 3648461 290154
All data are with sample of the same race, and three batch the data obtained averages are defined.
Drawn by above-mentioned data, the prepared rhizome of rehmannia stable content prepared by two suboptimum preparation technologies, with repeatability, Illustrate that experiment condition is objective, replica test result can be used as.
It can be drawn by testing two data, if processing temperature not enough, the generation of its active constituent content is not enough;If processing temperature Height is spent, its active ingredient declines rapidly, possible active ingredient is destroyed rapidly by high temperature, if being charred, secondary medicine is all by the gross Destroy, otherwise not only without drug effect, or even have harmful components generation.
In summary, proposition of the invention, is of great significance for the optimal concocting method tool for setting up prepared rhizome of rehmannia. It is specific to quantify, set up standard practice instructions(SOP)It is that the performance of its main body drug effect is established to ensure the fine quality of prepared rhizome of rehmannia Basis.The yield and quality of glutinous rehmannia are improved, glutinous rehmannia resource is preferably rationally utilized, enables it to play bigger curative effect, greatly Improve Business Economic Benefit.
The above described is only a preferred embodiment of the present invention, being not the limitation for making other forms to the present invention, appoint What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc. Imitate embodiment.But it is every without departing from technical solution of the present invention content, the technical spirit according to the present invention is to above example institute Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.

Claims (10)

1. the nine of a kind of prepared rhizome of rehmannia steam nine concocting methods processed, it is characterised in that including:
The first step, selection;
Second step, wash;
3rd step, one, which steams one, makes;
4th step, two, which steam two, makes;
5th step, three, which steam three, makes;
6th step, four, which steam four, makes;
7th step, five, which steam five, makes;
8th step, six, which steam six, makes;
9th step, seven, which steam seven, makes;
Tenth step, eight, which steam eight, makes;
11st step, nine, which steam nine, makes;
12nd step, sterilizing, packaging.
2. the nine of prepared rhizome of rehmannia as claimed in claim 1 steam nine concocting methods processed, it is characterised in that:Nine steam nine in the concocting method The temperature range of prepared rhizome of rehmannia processed is 130 DEG C~150 DEG C.
3. the nine of prepared rhizome of rehmannia as claimed in claim 1 or 2 steam nine concocting methods processed, it is characterised in that:Nine in the concocting method The pressure limit for steaming nine-processing radix rehmanniae preparata is 0.2Mpa~0.4Mpa.
4. the nine of prepared rhizome of rehmannia steam nine concocting methods processed as described in claims 1 to 3, it is characterised in that:Nine in the concocting method The mass ratio of radix rehmanniae recen to be processed and yellow rice wine is 3 used in steaming nine-processing radix rehmanniae preparata:1~2:1.
5. the nine of prepared rhizome of rehmannia steam nine concocting methods processed as described in Claims 1-4, it is characterised in that:3rd step is further Specially:
A is walked, and the radix rehmanniae recen after net system is placed in Turnround basket by infusing drugs in wine, plus yellow rice wine, and yellow rice wine amount is the 20% of total yellow rice wine addition ~25% is advisable, and infiltration is sucked for 2~4 hours to wine, and half an hour is stirred once;
B is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, middle product are put into tilting-type digester or uniformly inserted in food steamer, the steaming that pressure is 0.2~0.4Mpa is passed through Vapour stops steam one night of vexed profit for about 8 hours, steams to inside and outside in black is moistened, pours out liquid and prepared rhizome of rehmannia that the inside is steamed;
C is walked, and prepared rhizome of rehmannia is dried:Temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
D is walked, and is mixed, and mixes first time distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary, obtain middle product.
6. the nine of prepared rhizome of rehmannia steam nine concocting methods processed as described in claim 1 to 5, it is characterised in that:4th step is further Specially:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 6 hours, stops the vexed profit of steam 2 hours, pours out liquid and prepared rhizome of rehmannia that the inside is steamed;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes second of distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
7. the nine of prepared rhizome of rehmannia steam nine concocting methods processed as described in claim 1 to 6, it is characterised in that:5th step is further Specially:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, by middle product put into tilting-type digester in or uniformly insert in food steamer, supplement yellow rice wine, be passed through pressure be 0.2~ 0.4Mpa steam about 4 hours, stops the vexed profit of steam 2 hours, pours out liquid and prepared rhizome of rehmannia that the inside is steamed;
B is walked, and prepared rhizome of rehmannia is dried, and temperature is 55~60 DEG C, dry about 36 hours to eighty per cant it is dry or spread out and made naturally near in field processed It is dry;
C is walked, and is mixed, and mixes third time distillate and dried prepared rhizome of rehmannia thoroughly infiltration about 2~4 hours, half an hour stirs one It is secondary.
8. the nine of prepared rhizome of rehmannia steam nine concocting methods processed as described in claim 1 to 7, it is characterised in that:11st stepping one Step is specially:
A is walked, and is steamed, and is performed《Steam post standard practice instructions》And《Digester standard practice instructions》Or《Food steamer standard is grasped Make code》, middle product are put into tilting-type digester or uniformly inserted in food steamer, yellow rice wine is supplemented, yellow rice wine addition is total yellow The 20%~25% of wine addition is advisable, and is passed through the steam 4 hours that pressure is 0.2~0.4Mpa, stops the vexed profit of steam 2 hours, pours out The liquid and prepared rhizome of rehmannia that the inside is steamed are mixed thoroughly;
B walk, prepared rhizome of rehmannia dry, temperature be 55~60 DEG C, dry 36 hours to six, seventy percent it is dry or spread out in field processed dry in the air naturally make extremely 6th, seventy percent is dry;
C is walked, and is dried, and is performed《Dry post standard practice instructions》,《Heated-air circulation oven standard practice instructions》Or《Opened type Baking oven standard practice instructions》, 55~60 DEG C of design temperature, product prepared rhizome of rehmannia 25~30mm of thickness is 36 hours time, dried Moisture is controlled within 15.0 ﹪.
9. the prepared rhizome of rehmannia prepared using claim 1 to 8 methods described.
10. prepared rhizome of rehmannia as claimed in claim 9, it is characterised in that:HMF detects that peak area is preferred through HPLC in the prepared rhizome of rehmannia 3500000~3700000, HMFA detect peak area preferably 280000~300000 through HPLC.
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CN108175803A (en) * 2018-03-12 2018-06-19 汕头市粤东药业有限公司 A kind of processing procedure of prepared rehmannia root
CN108186850A (en) * 2018-03-12 2018-06-22 汕头市粤东药业有限公司 A kind of wine desert cistanche processing procedure
CN108783154A (en) * 2018-06-26 2018-11-13 成都煜泉绿健科技有限公司 A kind of Siberian solomonseal rhizome health-care functional beverage
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CN109876056A (en) * 2019-04-23 2019-06-14 漳州市老奇方商贸有限公司 A kind of preparation method being different from traditional nine radix rehmanniae preparatas processed
CN110237148A (en) * 2019-07-22 2019-09-17 河南尚华堂药业股份有限公司 A kind of Rehmannia glutinosa production technology
CN110522818A (en) * 2019-10-15 2019-12-03 安徽协和成药业饮片有限公司 A kind of concocting method of Rehmannia glutinosa medicine materical crude slice
CN113144094A (en) * 2021-05-26 2021-07-23 云南摩都农业有限责任公司 Method and device for processing polygonatum sibiricum by nine steaming
CN113350407A (en) * 2021-04-21 2021-09-07 安徽华善堂中药饮片有限公司 Processing technology of nine-steamed nine-processed pericarpium citri reticulatae traditional Chinese medicine decoction pieces
CN116196358A (en) * 2022-12-13 2023-06-02 山西广誉远国药有限公司 Rehmannia root nine-steaming nine-sun processing method and quality detection system

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CN107929418A (en) * 2017-10-25 2018-04-20 安徽华善堂中药饮片有限公司 A kind of nine steam the technological process of nine-processing radix rehmanniae preparata
CN108175803A (en) * 2018-03-12 2018-06-19 汕头市粤东药业有限公司 A kind of processing procedure of prepared rehmannia root
CN108186850A (en) * 2018-03-12 2018-06-22 汕头市粤东药业有限公司 A kind of wine desert cistanche processing procedure
CN108783154A (en) * 2018-06-26 2018-11-13 成都煜泉绿健科技有限公司 A kind of Siberian solomonseal rhizome health-care functional beverage
CN108938812A (en) * 2018-08-23 2018-12-07 陕西广济堂医药集团股份有限公司 A kind of production method of Rehmannia glutinosa purification medicine materical crude slice
CN109876056A (en) * 2019-04-23 2019-06-14 漳州市老奇方商贸有限公司 A kind of preparation method being different from traditional nine radix rehmanniae preparatas processed
CN110237148A (en) * 2019-07-22 2019-09-17 河南尚华堂药业股份有限公司 A kind of Rehmannia glutinosa production technology
CN110522818A (en) * 2019-10-15 2019-12-03 安徽协和成药业饮片有限公司 A kind of concocting method of Rehmannia glutinosa medicine materical crude slice
CN113350407A (en) * 2021-04-21 2021-09-07 安徽华善堂中药饮片有限公司 Processing technology of nine-steamed nine-processed pericarpium citri reticulatae traditional Chinese medicine decoction pieces
CN113144094A (en) * 2021-05-26 2021-07-23 云南摩都农业有限责任公司 Method and device for processing polygonatum sibiricum by nine steaming
CN116196358A (en) * 2022-12-13 2023-06-02 山西广誉远国药有限公司 Rehmannia root nine-steaming nine-sun processing method and quality detection system

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