Background technology
Fructus Alpiniae Oxyphyllae is the mature fruit of zingiberaceous plant Fructus Alpiniae Oxyphyllae Alpinia oxyphylla Miq..Be the tcm clinical practice medicinal herbs most in use.
Ancient times, the concocting method of Fructus Alpiniae Oxyphyllae was fairly simple, and the process of preparing Chinese medicine of giving birth to Fructus Alpiniae Oxyphyllae is shelled in the book on Chinese herbal medicine in ancient times and do not shelled two kinds of records.That advocates to shell has " celestial being is awarded the treating trauma and fracture secret recipe ", " precious mirror of hygiene ", " book on Chinese herbal medicine covers and signs ", " Bencao Pinhui Jingyao " etc., and this is a main flow, and that does not advocate to shell has " Prescriptions for Universal Relief " etc." peeling is fried ", " shelling " in Tang's " celestial being is awarded the treating trauma and fracture secret recipe ", have been put down in writing earlier.The record of " control married woman's metrorrhagia, the stir-fry of Fructus Alpiniae Oxyphyllae is fine ground, and drink is not gone into the salt clothes " is also arranged in " producing treasured through imitating " thereafter,, then develop into salt and fry together, be intended to bring into play the specially capable part of the body cavity below the umbilicus, housing the bladder, kidneys and bowels effect of salt because of this medicine is used for the warm part of the body cavity below the umbilicus, housing the bladder, kidneys and bowels more.Frying rule has to shell to fry and fries with Fructus Forsythiae that to get core not, all belongs to the meaning that relaxes the hot dry property of medicine.Song's " Shengji Zonglu " is carried: " peeling is fried.Control taste gas discord, do not eat." " Hong Shi collection proved recipe " at first mention " get core, salt fry "." Pu Ben " records stir-fry, and " hundred ask " mentions " beating broken ".Unit substitutes stir-fry, " salt water logging stir-fry " (" physicians from a family for generations "), thin usefulness (unit's methods such as " precious mirror " is smash in peeling.Bright " big gun is processed rule of treatment " mentions " stir-fry of shelling; face with grinding ", and the Ming Dynasty also has " salt stir-fry ", " water from washing rice soaks three places, dries ", " water logging goes out meat; Sucus Zingberis is fried " (" Prescriptions for Universal Relief ") in addition, " Prescriptions for Universal Relief " put down in writing the consumption of adjuvant salt simultaneously, says: " four liang, thumb is broken; two liang of salt; in porcelain, and order perfume is ripe with frying, and sifting out salt need not.It is smalls that Fructus Alpiniae Oxyphyllae is ground ", ", desalting " with two liang of stir-frys of salt; " shell; saline is fried; porphyrize (" protecting unit "); " special effect " records that Halitum wine boils, have in " bright doctor " processed with honey, " kindness " to mention that roasting, " Song Shi " saline are fried, " Jing Yue " also puts down in writing multiple concocting methods such as wine stir-fry; " illiteracy an aromatic plant metioned in ancient books " said: the charcoal processing process of preparing Chinese medicine method that " frying the black end that is " etc. do not add adjuvant is mentioned in " grindings ", " Synopsis of Treating Women's Diseases " first.The Qing Dynasty have stewing method (" hook unit "), salt wine fry (" collected explanations or commentaries "), system Fructus Alpiniae Oxyphyllae (clear " guide ", shell, grind methods such as (" saying pact ") into powder.The Qing Dynasty has clean system methods such as " discarding stalks " to record and narrate in addition.
To processing action and meaning that Fructus Alpiniae Oxyphyllae salt is fried, many doctor's nationalitys of Ming and Qing Dynasties all further are described." many urine person went into salt and tested with decoction is odd night as having put down in writing in bright " book on Chinese herbal medicine is taken advantage of refined partly brave ".Mention in " book on Chinese herbal medicine just " " be in harmony the seminal emission heeltap, red and white leukorrhea many urine person at turbid and night, get 20 surplus piece, grind salt a little, with decoction it, post and test ".Clearly " summary " have " urine reducing ... Fructus Alpiniae Oxyphyllae alite in Leizhou is fried, and desalts .... paste pill ", clear " guide " said: " Fructus Alpiniae Oxyphyllae salt is fried, and ends frequent micturition ".Clearly " jade is seized " shell fry grind help digestion the best." book on Chinese herbal medicine cover bamboo fish trap " has that " the preventing or arresting vomiting sound of vomiting and take the photograph saliva and spittle transfers all gas with the peace three warmers.More control and urinate night more, the decoction of people's salt is had immediate effect " record.
The concocting method in modern age mainly is the method for inheriting in ancient times.But the method for parch and purpose seemingly have certain difference at all times, and be to grind usefulness after shelling ancient times one, the one, and usefulness is fried in the back of shelling, and this uses and ripe usefulness for the life of Fructus Alpiniae Oxyphyllae.It is existing that " Chinese pharmacopoeia is recorded the decoction pieces specification of two kinds of concocting methods of Fructus Alpiniae Oxyphyllae Renhe stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution.
Because commodity are fruit (name Fructus Alpiniae Oxyphyllaes), the clinical requirement again with seed (name Fructus Alpiniae Oxyphyllae), so method now is to shell after the Fructus Alpiniae Oxyphyllae of band shell is fried to get core, the main purpose of parch is in order to shell, and is not direct parch seed.It mainly is to stay core to shell that Fructus Alpiniae Oxyphyllae at present is used as medicine.Fructus Alpiniae Oxyphyllae is shelled, and traditional method is to smash to pieces in stone mortar or grind broken in mill groove.
All parts of the country still have " removing impurity and shell; the time spent smashs to pieces ", " salt is processed ", intense fire to fry to brown, grinding at present, remove crust, get core slow fire and fry, spray saline to little yellow, fry to do, method for makings such as " Fructus Alpiniae Oxyphyllae is shelled, saline stirs; fry to showing heat color, spray saline is fried little doing ", " saline steams half an hour ", " processed with honey ", " fry to shell and be burnt brown; heave, kernel is yellow ", " stir-baking in sand "." pharmacopeia " adopts now; Be the method that mixes the back parch earlier,, have shell usefulness, the product of giving birth to of livings product to be with shell usefulness because the concocting method successive dynasties disunity of Fructus Alpiniae Oxyphyllae has not yet to see objective unified process of preparing Chinese medicine kind and processing procedure; Salt is processed the traditional processing procedure operation of product and how to be carried out, to lack unified technical data with pharmaceutical worker's experience; the product quality evaluation is based on sense organ; mostly be qualitative description; lack quantitative internal control index parameter; cause product quality uneven; influence clinical effectiveness, be difficult to adapt to large-scale production and growing medication demand.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art structure, the invention provides a kind of Fructus Alpiniae Oxyphyllae Chinese medicinal preparation method.
The technical scheme that technical solution problem of the present invention is adopted is:
A kind of Fructus Alpiniae Oxyphyllae Chinese medicinal preparation method, contain following steps:
(1) Fructus Alpiniae Oxyphyllae (Fructus Alpiniae Oxyphyllae shell technology): get clean Fructus Alpiniae Oxyphyllae 15kg, drop into the medicine roasting machine interior (about 220 ℃ of temperature) of preheating, moderate heat heating, the medicine roasting machine internal surface temperature is controlled at 290 ℃--320 ℃, Fructus Alpiniae Oxyphyllae medical material surface temperature control is at 160 ℃--170 ℃, about 7-8min of parch time, take the dish out of the pot rapidly when cracker reduces, airing, treat cold after, with its grating, selecting crude drugs with winnower eliminates shell with flattening mill; Packing;
(2) Fructus Alpiniae Oxyphyllae salt is processed technology: get clean Fructus Alpiniae Oxyphyllae, add 30% saline solution (concentration is 6.67%), mix thoroughly, profit 20min puts the medicine roasting machine interior (about 150 ℃ of temperature) of preheating, the slow fire heating, the medicine roasting machine internal surface temperature is controlled at 170 ℃--and 180 ℃, the Fructus Alpiniae Oxyphyllae surface temperature control is at 70 ℃--and 75 ℃, about 5-6min of parch time, take the dish out of the pot airing rapidly; Treat cold after, the packing.
Temperature, Fructus Alpiniae Oxyphyllae medical material surface temperature record for the Non-contact Infrared Temperature Measurement rifle in the medicine roasting machine;
A kind of Fructus Alpiniae Oxyphyllae Chinese medicine assay method, contain following steps:
The preparation process of sample liquid:
It is an amount of to get living Fructus Alpiniae Oxyphyllae, beats powder through pulverizer and crosses 30 mesh sieves, obtains Sharpleaf Glangal Fruit, places the wide mouthed bottle of clean dried, and standby behind the good seal.
Get about 2 grams of living Fructus Alpiniae Oxyphyllae sample powder, place the 250ml round-bottomed flask, add the defat with petroleum ether 1h of 60-90 ℃ of boiling range of 15 times of amounts earlier, filter.Add the defat with petroleum ether 0.5h of 60-90 ℃ of boiling range of 12.5 times of amounts in the filtering residue again, filter.Filtering residue places former round-bottomed flask together with filter paper, adds the alcohol reflux 2h of 25 times of amounts 80% again, filters, and adds 80% alcohol reflux 1h of 20 times of amounts in the filtering residue again, filters, and filtering residue alcohol is washed, merge extractive liquid,, sucking filtration.Filtrate is transferred in the clean round-bottomed flask, reclaims ethanol.Evaporate to dryness, reuse 80% dissolve with ethanol filters, and shifts fully and put in the 100ml volumetric flask, and reuse 80% ethanol standardize solution promptly gets sample liquid.
Determination step:
Precision pipettes sample solution 3.0ml and puts in the 25ml volumetric flask, adds 5%NaNO respectively
2And 10%AlCl
3Each 1.0ml leaves standstill 6min.Add 10%NaOH10.0ml again, add water to scale and shake up back placement 5min.And do blank with 80% ethanol, measure down in 510nm.
Beneficial effect of the present invention is specific as follows:
The present invention determines the technical data of the shell technology and the processed with salt of Fructus Alpiniae Oxyphyllae, sets up the pilot scale production technology of Fructus Alpiniae Oxyphyllae, two kinds of decoction pieces of processed with salt Fructus Alpiniae Oxyphyllae.
Process the pharmacodynamic study of Fructus Alpiniae Oxyphyllae by Fructus Alpiniae Oxyphyllae, salt, find that first Fructus Alpiniae Oxyphyllae and salt processs Fructus Alpiniae Oxyphyllae and all can significantly strengthen mice tolerance to cold and anti-fatigue ability animal stress and " yang deficiency syndrome ", " yin deficiency syndrome " mouse immune organ weight influence; Significantly increase the immune organ weight of yang deficiency and deficiency of YIN mice.Prompting Fructus Alpiniae Oxyphyllae and salt are processed the effect that Fructus Alpiniae Oxyphyllae has certain tonifying YANG, sets upright tonify deficiency.Be tcm clinical practice medication outline scientific basis.
Adopt scopolamine to cause rat memory acquisition disturbance model, observe of the influence of Fructus Alpiniae Oxyphyllae water extract by behavioral experiment to learning and memory in rats, and be index with acetylcholinesterase vigor and Hippocampus brain protein content, inquired into the Fructus Alpiniae Oxyphyllae water extract to improving the effect of learning memory disorder; The result shows, 1, the Fructus Alpiniae Oxyphyllae water extract is to the influence of dysmnesia learning and memory in rats ability due to the scopolamine: the basic, normal, high dosage group of Fructus Alpiniae Oxyphyllae required frequency of training up to standard significantly is lower than model group [(58.6 ± 15.0,55.0 ± 13.8,67.6 it is ± 8.7) inferior, (136.3 ± 16.8) are inferior, (p≤0.01)], model group rat required frequency of training up to standard is significantly higher than matched group (p≤0.01).2, the Fructus Alpiniae Oxyphyllae water extract is to the influence of dysmnesia rat hippocampus acetylcholinesterase vigor due to the scopolamine: Fructus Alpiniae Oxyphyllae low dose group and middle dosage group Hippocampus acetylcholinesterase vigor significantly are lower than model group (28.5 ± 9.3,22.2 ± 7.2) uka t/g, (47.2 ± 18.8) uka t/g, (p≤0.05).Model group Hippocampus acetylcholinesterase vigor is significantly higher than matched group (p≤0.05).3, the Fructus Alpiniae Oxyphyllae water extract is to the influence of dysmnesia rat hippocampus brain protein content due to the scopolamine: compare with model group, Fructus Alpiniae Oxyphyllae low dose group, middle dosage group brain protein content significantly increase (p≤0.05); Compare with matched group, model group rat hippocampus brain protein content significantly reduces (p≤0.05).Confirm that the Fructus Alpiniae Oxyphyllae water extract can improve laboratory animal study memory ability, has nootropic effect preferably.Thereby show Fructus Alpiniae Oxyphyllae water extract acetylcholine esterase inhibition activity, reduce acetylcholine and decompose, improve Hippocampus brain protein content, memory acquisition disturbance due to the scopolamine is had significant improvement effect.For clinical Fructus Alpiniae Oxyphyllae treatment study memory acquisition disturbance disease provides experimental basis.
The present invention has studied Fructus Alpiniae Oxyphyllae, salt and has processed the influence of Fructus Alpiniae Oxyphyllae to animal stress and " yang deficiency syndrome ", " yin deficiency syndrome " mouse immune organ weight.The result is as follows:
(1) to the influence of animal stress
1, purpose
Observation Fructus Alpiniae Oxyphyllae, salt are processed the influence of Fructus Alpiniae Oxyphyllae gastric infusion to mice tolerance to cold and anti-fatigue ability.
2, material
Kunming mouse 20g ± 2g provides (quality certification number: the Anhui doctor real moving accurate 01) by the Anhui Chinese Medicine College Experimental Animal Center.
Fructus Alpiniae Oxyphyllae, salt are processed the Fructus Alpiniae Oxyphyllae water extract, self-control, and every 1ml is equivalent to 0.5g Fructus Alpiniae Oxyphyllae medical material.
3, experimental technique
3.1 grouping and administration
60 of Kunming mouses, male, body weight 18-22g is divided into 3 groups at random by body weight, is respectively normal group, Fructus Alpiniae Oxyphyllae group, salt and processs the Fructus Alpiniae Oxyphyllae group.Fructus Alpiniae Oxyphyllae group, salt process Fructus Alpiniae Oxyphyllae group mice by the 0.1ml/10g body weight irritate the stomach Fructus Alpiniae Oxyphyllae respectively, salt is processed the Fructus Alpiniae Oxyphyllae water extract, normal group is irritated stomach contrast, successive administration 7 days with normal saline.Experimentized in 1 hour after the last administration.
3.2 statistical analysis
Data are all with means standard deviation
Expression adopts SPSS11.5 software to carry out analyzing and processing.
4, result
4.1 influence (20 ℃ of room temperatures) to the mouse anti-reflecting fatigue ability
Get 10 of mices respectively from three groups, respectively get 2 of mices from three groups at every turn, the container of putting into 25 ℃ of water temperatures, depth of water 50cm simultaneously allows mice swimming, is index to be drowned, the record mice from entry to the dead time.The result is as follows:
Table 1 Fructus Alpiniae Oxyphyllae is to the influence of mice swimming time
Annotate: compare with normal group,
*P<0.01.
The result shows that Fructus Alpiniae Oxyphyllae and salt are processed Fructus Alpiniae Oxyphyllae and all can be swum in the water and the time-to-live by the significant prolongation mice; Wherein salt product is longer than the product of the giving birth to prolongation mice time-to-live, but both differences do not have significance.Show that both all have the ability that strengthens mouse anti-reflecting fatigue.
4.2 influence (25 ℃ of room temperatures) to the mice cold tolerance
Getting 10 of mices respectively from three groups, respectively get 2 of mices from three groups at every turn, put into temperature simultaneously and be 4 ℃ frozen water, is index to be drowned, the time of record mice survival.The result is as follows:
Table 2 result shows that Fructus Alpiniae Oxyphyllae and salt are processed equal energy significant prolongation mice time-to-live in frozen water of Fructus Alpiniae Oxyphyllae; Wherein salt product is longer than the product of the giving birth to prolongation mice time-to-live, but both differences do not have significance.Show that both all have the cold-resistant ability of the mice of enhancing.
Table 2 Fructus Alpiniae Oxyphyllae is to the influence of mice tolerance to cold
Annotate: compare with normal group,
*P<0.05,
*P<0.01.
(2) to the influence of experimental " yang deficiency syndrome " animal
1, purpose
Observe Fructus Alpiniae Oxyphyllae and salt and process of the influence of Fructus Alpiniae Oxyphyllae gastric infusion the immune organ weight of hydrocortisone inductive " yang deficiency syndrome " model mice.
2, material
Kunming mouse 20g ± 2g provides (quality certification number: the Anhui doctor real moving accurate 01) by the Anhui Chinese Medicine College Experimental Animal Center.
Fructus Alpiniae Oxyphyllae and salt are processed the Fructus Alpiniae Oxyphyllae water extract, self-control, and every 1ml is equivalent to 0.5g Fructus Alpiniae Oxyphyllae medical material.
Hydrocortisone injection, Xi'an Lijun pharmaceutical Co., Ltd's product, lot number: 050405;
3, experimental technique
3.1 grouping and administration
40 of Kunming mouses, male, body weight 18-22g is divided into 4 groups at random by body weight, is respectively normal group, hydrocortisone model group, Fructus Alpiniae Oxyphyllae group and salt product group.Fructus Alpiniae Oxyphyllae and salt product group mice are irritated the stomach Fructus Alpiniae Oxyphyllae respectively by the 0.1ml/10g body weight and give birth to product and salt product water extract, and normal group and model group be respectively with physiologic saline for substitute, continuous irrigation stomach 10 days.Experimentized in 1 hour after the last administration.
3.2 modeling method
During experiment, except that normal group, other respectively organize mice self administration of medication the 4th day beginning simultaneously every by 0.5mg/0.1ml intragluteal injection hydrocortisone injection, the normal saline of normal group injection respective volume, continuous 6 days.Claim the mice body weight during experiment earlier, take off cervical vertebra then and put to death mice, get spleen, thymus and adrenal gland, weigh, calculate each organ index.
3.3 statistical analysis
Data are all with means standard deviation
Expression adopts SPSS11.5 software to carry out analyzing and processing.
4 results
The result of table 3 shows that hydrocortisone significantly descends mouse spleen index, thymus index and adrenal gland's index; And give Fructus Alpiniae Oxyphyllae can significantly raise thymus index and adrenal gland's index, give salt and process Fructus Alpiniae Oxyphyllae can significantly raise index and spleen index, thymus index and adrenal gland's index; And salt to process the product group bigger to each exponential increase rate than Fructus Alpiniae Oxyphyllae group, but difference does not have significance.
Table 3 Fructus Alpiniae Oxyphyllae to hydrocortisone cause " yang deficiency syndrome " mouse immune organ weight influence (n=10,
)
Annotate: compare with normal group,
##P<0.01,
#P<0.05; Compare with model group,
*P<0.05,
*P<0.01.
(3) to the influence of experimental " yin deficiency syndrome " animal
1, purpose
Observe Fructus Alpiniae Oxyphyllae and salt and process of the influence of Fructus Alpiniae Oxyphyllae gastric infusion the inductive mice of thyroid tablet " yin deficiency syndrome " model.
2, material
Kunming mouse 20g ± 2g provides (quality certification number: the Anhui doctor real moving accurate 01) by the Anhui Chinese Medicine College Experimental Animal Center.
Fructus Alpiniae Oxyphyllae and salt are processed the Fructus Alpiniae Oxyphyllae water extract, self-control, and every 1ml is equivalent to 0.5g Fructus Alpiniae Oxyphyllae medical material.
Thyroid tablet, Shanghai Industrial United Holdings Great Wall Pharmaceutical Co., Ltd.'s product, lot number: 20050601;
3, experimental technique
3.1 grouping and administration
40 of Kunming mouses, male, body weight 18-22g is divided into 4 groups at random by body weight, is respectively normal group, thyroid tablet model group, Fructus Alpiniae Oxyphyllae and salt and processs the Fructus Alpiniae Oxyphyllae group.Product are given birth in Fructus Alpiniae Oxyphyllae and salt product group mice is irritated stomach Fructus Alpiniae Oxyphyllae life product and salt product water extract respectively by the 0.1ml/10g body weight, and normal group and model group be respectively with physiologic saline for substitute, continuous irrigation stomach 10 days.Experimentized in 1 hour after the last administration.
3.2 modeling method
During experiment, except that normal group, other respectively organize mice self administration of medication the 4th day beginning simultaneously every irritate 0.5% carboxymethylcellulose sodium solution that stomach gives thyroid tablet by 3mg/0.2ml, normal group gives 0.5% carboxymethylcellulose sodium solution of respective volume, once a day, continuous 6 days.Claim the mice body weight during experiment earlier, take off cervical vertebra then and put to death mice, get spleen, thymus and adrenal gland, weigh, calculate each organ index.
3.3 statistical analysis
Data are all with means standard deviation
Expression adopts SPSS11.5 software to carry out analyzing and processing.
4 results
The result of table 4 shows that thyroid can make mouse spleen index, thymus index and adrenal gland's index significantly descend; Process Fructus Alpiniae Oxyphyllae all can significantly raise index and spleen index, thymus index and the adrenal gland's index of mice and give Fructus Alpiniae Oxyphyllae and salt; And the Fructus Alpiniae Oxyphyllae group to process the Fructus Alpiniae Oxyphyllae group than salt big to the increase rate of index and spleen index and thymus index, and both differences that influence of thymus index are had significance; And salt is processed the Fructus Alpiniae Oxyphyllae group to the living product height of the exponential raising of adrenal gland, but both differences do not have significance.
Table 4 Fructus Alpiniae Oxyphyllae to " yin deficiency syndrome " mouse immune organ weight's influence (n=10,
)
Annotate: compare with normal group,
##P<0.01,
#P<0.05; Compare with model group,
*P<0.05,
*P<0.01; Compare with Fructus Alpiniae Oxyphyllae processed with salt group,
△P<0.05.
(4) conclusion
Fructus Alpiniae Oxyphyllae and salt are processed Fructus Alpiniae Oxyphyllae all can significantly strengthen mice tolerance to cold and anti-fatigue ability; Significantly increase the immune organ weight of yang deficiency and deficiency of YIN mice.Prompting Fructus Alpiniae Oxyphyllae and salt are processed the effect that Fructus Alpiniae Oxyphyllae has certain tonifying YANG, sets upright tonify deficiency.The further research and confirming but these effects are still needed is as its influence to the stress abilities such as ability of animal high temperature resistance, anti-hypobaric hypoxia, to the influence of animal function etc.
The specific embodiment
A kind of Fructus Alpiniae Oxyphyllae Chinese medicinal preparation method, contain following steps:
(1) Fructus Alpiniae Oxyphyllae (Fructus Alpiniae Oxyphyllae shell technology): get clean Fructus Alpiniae Oxyphyllae 15kg, drop into the medicine roasting machine interior (about 220 ℃ of temperature) of preheating, moderate heat heating, the medicine roasting machine internal surface temperature is controlled at 290 ℃--320 ℃, Fructus Alpiniae Oxyphyllae medical material surface temperature control is at 160 ℃--170 ℃, about 7-8min of parch time, take the dish out of the pot rapidly when cracker reduces, airing, treat cold after, with its grating, selecting crude drugs with winnower eliminates shell with flattening mill; Pack the 0.5kg/ bag with plastic bag airtight package and kraft paper respectively again;
Temperature, Fructus Alpiniae Oxyphyllae medical material surface temperature record for the Non-contact Infrared Temperature Measurement rifle in the medicine roasting machine;
Every 100kg Fructus Alpiniae Oxyphyllae can make the about 67~70kg of Fructus Alpiniae Oxyphyllae.
(2) Fructus Alpiniae Oxyphyllae salt is processed technology: get clean Fructus Alpiniae Oxyphyllae, add 30% saline solution (concentration is 6.67%), mix thoroughly, profit 20min puts the medicine roasting machine interior (about 150 ℃ of temperature) of preheating, the slow fire heating, the medicine roasting machine internal surface temperature is controlled at 170 ℃--and 180 ℃, the Fructus Alpiniae Oxyphyllae surface temperature control is at 70 ℃--and 75 ℃, about 5-6min of parch time, take the dish out of the pot airing rapidly; Treat cold after, pack the 0.5kg/ bag with plastic bag airtight package and kraft paper respectively again.Yield 98.5%~102.5%.
Every 100kg Fructus Alpiniae Oxyphyllae 2kg Sal.
Temperature, Fructus Alpiniae Oxyphyllae medical material surface temperature record for the Non-contact Infrared Temperature Measurement rifle in the medicine roasting machine;
Pilot scale is 25% o'clock with the Sal water yield, because the medical material amount is big, can not mix thoroughly, influences its quality, through experiment, it is adjusted into 30%, after mixing, still has residual liquid not exhaust, and before the heating parch, need dry, and parch is better again.
A kind of Fructus Alpiniae Oxyphyllae Chinese medicine assay method, contain following steps:
The preparation process of sample liquid:
It is an amount of to get living Fructus Alpiniae Oxyphyllae, beats powder through pulverizer and crosses 30 mesh sieves, obtains Sharpleaf Glangal Fruit, places the wide mouthed bottle of clean dried, and standby behind the good seal.
Get about 2 grams of living Fructus Alpiniae Oxyphyllae sample powder, place the 250ml round-bottomed flask, add the defat with petroleum ether 1h of 60-90 ℃ of boiling range of 15 times of amounts earlier, filter.Add the defat with petroleum ether 0.5h of 60-90 ℃ of boiling range of 12.5 times of amounts in the filtering residue again, filter.Filtering residue places former round-bottomed flask together with filter paper, adds the alcohol reflux 2h of 25 times of amounts 80% again, filters, and adds 80% alcohol reflux 1h of 20 times of amounts in the filtering residue again, filters, and filtering residue alcohol is washed, merge extractive liquid,, sucking filtration.Filtrate is transferred in the clean round-bottomed flask, reclaims ethanol.Evaporate to dryness, reuse 80% dissolve with ethanol filters, and shifts fully and put in the 100ml volumetric flask, and reuse 80% ethanol standardize solution promptly gets sample liquid.
Determination step:
Precision pipettes sample solution 3.0ml and puts in the 25ml volumetric flask, adds 5%NaNO respectively
2And 10%AlCl
3Each 1.0ml leaves standstill 6min.Add 10%NaOH10.0ml again, add water to scale and shake up back placement 5min.And do blank with 80% ethanol, measure down in 510nm.