Background technology
Lepidinm meyenii Walp (Maca) is annual or 2 years SHENGCAO bases, storage root is arranged, paste short stem and the leaf of ground growth, originate in the mountain area, Andean, South America of 3500 ~ 4500 meters of height above sea level, at present China in Yunnan, Xinjiang successful introduction on a large scale, for Cruciferae (Cruciferae) separate row Vegetable spp (
Lepidium) plant.Lepidinm meyenii Walp is as medicine food dual purpose plant, and the underground tuber that expands is mainly to eat part, and surface color has black, purple, yellow etc.Lepidinm meyenii Walp rich in proteins, aminoacid, saccharide, mineral and multivitamin, the edible history in South America has had more than 5800 year, is used for traditionally strengthening body, improves fertility, improves sexual function, antidepressant, anti-anemia etc.After the eighties in 20th century, the recommendation through FAO (Food and Agriculture Organization of the United Nation) (FAO) and International Plant Genetic Resources Institute (IPGRI), the chemical composition of Lepidinm meyenii Walp is identified, active component separates and pharmacological action is furtherd investigate.Beginning of the nineties particularly, researcher has been found this kind of plant in the remarkable efficacy that improves on the sexual function when seeking " viagra " succedaneum, makes Lepidinm meyenii Walp become at one stroke nova in international health product and the medicine.A large amount of scientific researches show, Lepidinm meyenii Walp has resisting fatigue, improve sexual function, reduce the multiple efficacies such as prostatic hyperplasia, and nontoxic, edible safety.Most researcheres think that Lepidinm meyenii Walp amide (macamides), benzyl mustard oil glycosides (benzyl glucosinolate claims again glucotropaeolin) and its catabolite benzyl isothiocyanate (benzy is othiocyanates) are its main active and property material.Studies show that, the catabolite isosulfocyanate material of glucosinolate has antitumor action, can have the effects such as the learning and memory of improvement and raising Male sexual ability as agent for increasing testosterone level, should keep glucosinolate in the course of processing as far as possible.
Glucosinolate is also referred to as thioglycoside or is called for short sulfur glycosides (glucosinolate is called for short GS), and full name is (Z)-cis-N-hydroximinosulfateesers, is distinctive bioactive substance in the crucifer.Glucosinolate mainly comes from seven seed amino acids (alanine, leucine, isoleucine, valine, phenylalanine, TYR, tryptophan) and a series of side chain prolongs congener, difference according to its source amino acid precursor is divided into aliphatic, aromatic series and indole family three major types with glucosinolate.Glucosinolate since with the difference of R base kind more than 100 is arranged, comprise benzyl mustard oil glycosides and several indoles glucosinolate and fatty acid glucosinolate.The content of glucosinolate in fresh Lepidinm meyenii Walp tuber is about more than 1%, and content is about 0.65% in the Lepidinm meyenii Walp tuber of natural drying, and fibrous root content is up to approximately 1.65%, and blade also contains approximately 0.36%.
At present, that the preparation of Lepidinm meyenii Walp dried product is generally adopted is dry after natural drying, hot air drying, low-temperature vacuum drying, the steam deactivation, the technique such as dry behind drying and the microwave inactivation after the blanching deactivation, part is such as drying process behind steam deactivation, blanching deactivation, the microwave inactivation, though the goods glucosinolate content that obtains improves, there is the problem of useful heat-sensitive substance such as protein inactivation, volatile ingredient minimizing, characteristic chemical constituent oxidation.The glucosinolate content of the Lepidinm meyenii Walp goods that most of conventional process drying obtains is far below fresh Lepidinm meyenii Walp.
The technology for extracting effective component of a large amount of scholar's research Lepidinm meyenii Walp, how research extracts glucosinolate and best catabolite, but the result often runs counter to desire, and glucosinolate and catabolite are lower than the content in the Lepidinm meyenii Walp raw material on the contrary in the extract, causes the active awkward result not as former powder of extract.The research institution of Japan thinks that bacillus bifidus and organized enzyme in the human digestive road can play unrivaled optimization Degradation in the digest and decompose glucosinolate, its catabolite composition also just people with artificial condition was difficult to obtain.So what the inventor thought that we will do is the Lepidinm meyenii Walp raw material that obtains ecosystem, keeps the unlikely degraded in processing, storage of its effective active composition, volatilization and destruction as far as possible.Pueraria root powder of developing so a kind of abundant retains biological activity and preparation method thereof is necessary with preparation.
Summary of the invention
The first purpose of the present invention is to provide a kind of pueraria root powder of abundant retains biological activity, and the second purpose is to provide the preparation method of this pueraria root powder, and the 3rd purpose is to provide the preparation of this pueraria root powder.
The first purpose of the present invention is achieved in that take fresh Lepidinm meyenii Walp as raw material, and through the pueraria root powder of freezing, lyophilization, pulverizing process preparation, the moisture content of described pueraria root powder wherein contains the glucosinolate that accounts for pueraria root powder gross weight 1.1 ~ 2.7% below 5%.
The second purpose of the present invention is achieved in that and comprises pre-treatment, freezing, lyophilization, pulverizing process, specifically comprises:
A, pre-treatment: with fresh Lepidinm meyenii Walp remove impurity, clean and dry surface moisture;
B, freezing: the Lepidinm meyenii Walp after the pre-treatment is packed in the refrigerating plant, freezing below-20 ℃;
C, lyophilization: the Lepidinm meyenii Walp that freezes is packed in the vacuum freezing drying device, behind pre-freeze, sublimation drying, parsing-desiccation, obtain the dried active Lepidinm meyenii Walp;
D, pulverizing: the Lepidinm meyenii Walp after the lyophilization obtains object after crushed.
The 3rd purpose of the present invention is achieved in that the adjuvant that the pueraria root powder adding pharmaceutical field of described abundant retains biological activity is accepted is prepared into tablet, powder, electuary or capsule.
Preparation method of the present invention adopts vacuum freeze-drying technique, suppressed the activity of myrosin in storage and dry run in the Lepidinm meyenii Walp, pass through simultaneously the ice crystal of moisture content in the Lepidinm meyenii Walp, destroy the condition of myrosin and glucosinolate generation hydrolysis, cold drying has also reduced the oxidation of Lepidinm meyenii Walp active component, make fresh Lepidinm meyenii Walp in dry run, keep to greatest extent property material (glucosinolate), protozoa active component such as protein and other volatile ingredient, reduced the glucosinolate hydrolyzate isosulfocyanate that contains penetrating odor and the generation of nitriles substance, the glucosinolate of reservation easily is decomposed into useful isothiocyanate isoreactivity effective ingredient by the microorganism in the intestinal and bacterial enzyme; By under the freezing state to dry after the Lepidinm meyenii Walp tuber section, both improved cryodesiccated efficient, guaranteed in the slicing processes glucosinolate not can with myrosin generation hydrolysis.The present invention makes the abundant retains biological activity of Lepidinm meyenii Walp active product and excellent flavor, the color and luster nature; Dried Lepidinm meyenii Walp active product is loose porous, is spongy, and as easy as rolling off a log and Digestive system merges, therefore.The present invention can fully utilize Lepidinm meyenii Walp tuber, fibrous root, leaf, particularly to the utilization of Lepidinm meyenii Walp fibrous root, Effective Raise the utilization rate of Lepidinm meyenii Walp.
The specific embodiment
The present invention is further illustrated below in conjunction with drawings and Examples, but never in any form the present invention is limited, and any change or improvement based on training centre of the present invention is done all belong to protection scope of the present invention.
The pueraria root powder of abundant retains biological activity of the present invention is as raw material take fresh Lepidinm meyenii Walp, prepare pueraria root powder through freezing, lyophilization, pulverizing process, the moisture content of described pueraria root powder wherein contains the glucosinolate that accounts for pueraria root powder gross weight 1.1 ~ 2.7% below 5%.
Described Lepidinm meyenii Walp is more than one in Lepidinm meyenii Walp tuber, Lepidinm meyenii Walp fibrous root, the Lepidinm meyenii Walp leaf.
Described glucosinolate comprises benzyl mustard oil glycosides, methoxy-benzyl glucosinolate.
The method of the abundant retains biological activity pueraria root powder of preparation of the present invention comprises pre-treatment, freezing, lyophilization, pulverizing process, specifically comprises:
A, pre-treatment: with fresh Lepidinm meyenii Walp remove impurity, clean and dry surface moisture;
B, freezing: the Lepidinm meyenii Walp after the pre-treatment is packed in the refrigerating plant, freezing below-20 ℃;
C, lyophilization: the Lepidinm meyenii Walp that freezes is packed in the vacuum freezing drying device, behind pre-freeze, sublimation drying, parsing-desiccation, obtain the dried active Lepidinm meyenii Walp;
D, pulverizing: the Lepidinm meyenii Walp after the lyophilization obtains object after crushed.
The described Lepidinm meyenii Walp of A step is more than one in Lepidinm meyenii Walp tuber, Lepidinm meyenii Walp fibrous root, the Lepidinm meyenii Walp leaf, and described Lepidinm meyenii Walp tuber, Lepidinm meyenii Walp fibrous root, Lepidinm meyenii Walp leaf are finished pre-treatment, freezing, lyophilization, pulverizing process together or respectively, can both realize purpose of the present invention.
Described Lepidinm meyenii Walp tuber is cut at lower Lepidinm meyenii Walp tuber of freezing state≤thin slice of 10mm thickness after the B step is freezing, then fills the lyophilizing dish and enters the C step.
Can not in time cryodesiccatedly send to stored under refrigeration after the B step, refrigerated storage temperature is-20 ~-30 ℃, sends to the lyophilization of carrying out the C step when needing lyophilization.That is, for intermittently operated or disperse freezing concentrated drying, should send to first stored under refrigeration after finishing with fresh Lepidinm meyenii Walp is freezing, by the time can be dry the time, send to again lyophilization.
The described pre-freeze temperature of C step is below-30 ℃, and vacuum is 20 ~ 80Pa; The eutectic point of described sublimation drying is at-15 ~-28 ℃; 35 ~ 45 ℃ of the Lepidinm meyenii Walp central temperatures of described parsing-desiccation.Through the dried pueraria root powder of method of the present invention, compare with other drying meanss, can keep to greatest extent the ecosystem active component of fresh goods, such as Lepidinm meyenii Walp alkene, Lepidinm meyenii Walp amide, activated protein and active polysaccharide, organized enzyme, vitamin etc.Described vacuum freezing drying device adopts transmission of heat by contact, compound heating, the combination of one of nail-plate heating, radiation heating, microwave heating, infrared heating mode or any-mode is arranged.
The described pulverizing of D step is a kind of during Ordinary pulverization, superfine grinding or airflow counter-collision super-micro wall-broken are pulverized.
The preparation of abundant retains biological activity pueraria root powder of the present invention is that the adjuvant that the pueraria root powder adding pharmaceutical field of described abundant retains biological activity is accepted is prepared into tablet, powder, electuary or capsule.
Operation principle of the present invention:
Commercially available MAKA dry powder or the glucosinolate content in the extract are very low, and this is because the myrosin system in the Lepidinm meyenii Walp causes.The glucosinolate of Lepidinm meyenii Walp is present in the cytoplasmic vacuole, myrosin be it is generally acknowledged in the myrosin cell of the heterocyst body in each organ that only is present in dispersion, when tissue sustains damage (as pulverizing, overstock, cutting into slices), glucosinolate easily and myrosin meet and hydrolysis occur, produce the chemical compounds such as different sulphuric acid hydrocyanic ester, sulphuric acid hydrocyanic ester and fine class.Preparation method of the present invention adopts vacuum freeze-drying technique, suppressed the activity of myrosin in storage and dry run in the Lepidinm meyenii Walp, pass through simultaneously the ice crystal of moisture content in the Lepidinm meyenii Walp, destroy the condition of myrosin and glucosinolate generation hydrolysis, cold drying has also reduced the oxidation of Lepidinm meyenii Walp active component, make fresh Lepidinm meyenii Walp in dry run, keep to greatest extent property material (glucosinolate), protozoa active component such as protein and other volatile ingredient, reduced the glucosinolate hydrolyzate isosulfocyanate that contains penetrating odor and the generation of nitriles substance, the glucosinolate of reservation easily is decomposed into useful isothiocyanate isoreactivity effective ingredient by the microorganism in the intestinal and bacterial enzyme; By under the freezing state to dry after the Lepidinm meyenii Walp tuber section, both improved cryodesiccated efficient, guaranteed in the slicing processes glucosinolate not can with myrosin generation hydrolysis.
Embodiment 1
Get yellow ripe fresh Lepidinm meyenii Walp tuber and the fibrous root of Lijiang, yunnan non-polluted planting, reject stem and leaf, worm's ovum, disease tuber and fibrous root, separate tuber and fibrous root, the room temperature accelerated surface is air-dry after clear water is cleaned; Tuber and fibrous root are packed in the refrigerating plant together ,-30 ℃ lower freezing, freeze 3h; Lepidinm meyenii Walp tuber after freezing the finishing is cut into the thick thin slice of 4mm, sends into-20 ℃ of Cold storage in the refrigerators with the Lepidinm meyenii Walp fibrous root to be dried; Lepidinm meyenii Walp tuber thin slice and Lepidinm meyenii Walp fibrous root uniform spreading are loaded in the lyophilizing dish, in the transmission of heat by contact formula of packing into the freeze drying plant, after-40 ℃ pre-freeze, be evacuated to 50Pa, plait point is set carries out sublimation drying for-17 ℃, again with 40 ℃ of lower parsing-desiccations of material central temperature, until moisture content 5% obtains the dried active Lepidinm meyenii Walp; Behind Ordinary pulverization, make dry pueraria root powder.Get the dry pueraria root powder that makes, measure glucosinolate content in the dried active Lepidinm meyenii Walp by the tablets by HPLC-MS among the agricultural industry criteria NY/T1103.3-2006 of the People's Republic of China (PRC), measurement result is: glucosinolate accounts for 2.46% of dry pueraria root powder gross weight.
Embodiment 2
Get yellow ripe fresh Lepidinm meyenii Walp tuber, fibrous root and the blade of Lijiang, yunnan non-polluted planting, reject stem, Huang Ye, worm's ovum, disease tuber and fibrous root, separate tuber and fibrous root, the room temperature accelerated surface is air-dry after clear water is cleaned; Tuber, fibrous root and blade are packed in the refrigerating plant ,-40 ℃ lower freezing, freeze 2h; The tuber of freezing state is cut into the thick thin slice of 1mm, thin slice be loaded in the lyophilizing dish through freezing fibrous root, blade uniform spreading, pack in the radiant heating type freeze drying plant, after-40 ℃ pre-freeze, be evacuated to 60Pa, plait point-15 be set ℃ carry out sublimation drying, again with 45 ℃ of lower parsing-desiccations of material central temperature, until moisture content 3% obtains the dried active Lepidinm meyenii Walp; Form dry pueraria root powder through Ordinary pulverization and after crossing 400 eye mesh screens.Get the dry pueraria root powder that makes, measure glucosinolate content in the dried active Lepidinm meyenii Walp by the tablets by HPLC-MS among the agricultural industry criteria NY/T1103.3-2006 of the People's Republic of China (PRC), measurement result is: glucosinolate accounts for 2.13% of dry pueraria root powder gross weight.
Embodiment 3
Get the ripe fresh Lepidinm meyenii Walp tuber of black and the fibrous root of Lijiang, yunnan non-polluted planting, reject stem and leaf, worm's ovum, disease tuber and fibrous root, separate tuber and fibrous root, after clear water is cleaned, remove surperficial excessive moisture with dewaterer; Pack in the refrigerating plant ,-35 ℃ lower freezing, freeze 3h; Lepidinm meyenii Walp tuber after freezing is cut into the thick thin slice of 5mm, and fibrous root is sent into-25 ℃ of Cold storage in the refrigerators; Lepidinm meyenii Walp tuber thin slice and fibrous root uniform spreading through cold preservation are loaded in the lyophilizing dish, after-35 ℃ pre-freeze, the two sides of packing into has in the compound heating freeze drying plant of hot plate, be evacuated to 40Pa, plait point-20 is set ℃ carries out sublimation drying, again with 45 ℃ of lower parsing-desiccations of material central temperature, until moisture content 4% obtains the dried active Lepidinm meyenii Walp; Pulverize and sieve through 1000 eye mesh screens through the airflow counter-collision super-micro wall-broken and obtain dried active pueraria root powder (super-micro wall-broken powder).Get the dry pueraria root powder that makes, measure glucosinolate content in the dried active Lepidinm meyenii Walp by the tablets by HPLC-MS among the agricultural industry criteria NY/T1103.3-2006 of the People's Republic of China (PRC), measurement result is: glucosinolate accounts for 1.71% of dry pueraria root powder gross weight.
Embodiment 4
Get the ripe fresh Lepidinm meyenii Walp tuber of black of Lijiang, yunnan non-polluted planting and fibrous root, leaf, reject yellow leaf, rotten stem, worm's ovum, disease tuber and fibrous root, separate tuber volume fibrous root, low temperature dries up fast after clear water is cleaned; Tuber and fibrous root are packed in the refrigerating plant ,-25 ℃ lower freezing, freeze 5h; Blade is packed in the refrigerating plant ,-30 ℃ lower freezing, freeze 1h; Lepidinm meyenii Walp tuber after freezing is sliced into the thick thin slice of 8mm, then sends into-20 ℃ of Cold storage in the refrigerators with fibrous root, blade; Lepidinm meyenii Walp tuber thin slice, fibrous root, blade uniform spreading through cold preservation are loaded in the lyophilizing dish, after-30 ℃ pre-freeze, be incorporated with middle the having in the nail-plated heating freeze drying plant of two hot plates of many pieces of nails, be evacuated to 25Pa, plait point-27 is set ℃ carries out sublimation drying, again with the parsing-desiccation of 35 ℃ of material central temperatures, until moisture content 5% obtains the dried active Lepidinm meyenii Walp; Sieve through micronizing and through 200 eye mesh screens and to obtain the dried active pueraria root powder.Get the dry pueraria root powder that makes, measure glucosinolate content in the dried active Lepidinm meyenii Walp by the tablets by HPLC-MS among the agricultural industry criteria NY/T1103.3-2006 of the People's Republic of China (PRC), measurement result is: glucosinolate accounts for 1.1% of dry pueraria root powder gross weight.
Embodiment 5
Get the ripe fresh Lepidinm meyenii Walp tuber of purple and the fibrous root of Lijiang, yunnan non-polluted planting, reject stem and leaf, worm's ovum, disease tuber and fibrous root, separate tuber and fibrous root, after clear water is cleaned, remove surperficial excessive moisture with dewaterer; Lepidinm meyenii Walp tuber and fibrous root are packed in the refrigerating plant ,-50 ℃ lower freezing, freeze 1.5h; Tuber is cut into the Cold storage in the refrigerator that 10mm thin slice and fibrous root are sent into temperature-30 ℃ in the lump; With the Lepidinm meyenii Walp tuber thin slice after the cold preservation, place in the lyophilizing dish, after-35 ℃ pre-freeze, pack in the microwave heating freeze drying box, be evacuated to 60Pa, plait point-18 be set ℃ carry out sublimation drying, again with the parsing-desiccation of 45 ℃ of material central temperatures, until moisture content 4% obtains dried active Lepidinm meyenii Walp A; Fibrous root after the cold preservation is installed in the lyophilizing dish, through-30 ℃ of pre-freezes, is evacuated to 80Pa, plait point-15 is set ℃ carries out sublimation drying, again with the parsing-desiccation of 40 ℃ of material central temperatures, until moisture content 2% obtains dried active agate B.Dried active Lepidinm meyenii Walp A and B sieve through micronizing and through 100 eye mesh screens respectively, obtain dried active pueraria root powder A(tuber superfine powder) and dried active pueraria root powder B(fibrous root superfine powder).Get the dry pueraria root powder that makes, measure glucosinolate content in the dried active Lepidinm meyenii Walp by the tablets by HPLC-MS among the agricultural industry criteria NY/T1103.3-2006 of the People's Republic of China (PRC), measurement result is: glucosinolate accounts for 1.38% of dry pueraria root powder gross weight dried active pueraria root powder A(tuber superfine powder); With dried active pueraria root powder B(fibrous root superfine powder) in glucosinolate account for 2.7% of dry pueraria root powder gross weight.
Embodiment 6
Get the ripe fresh Lepidinm meyenii Walp tuber of purple and the fibrous root of Lijiang, yunnan non-polluted planting, reject stem and leaf, worm's ovum, disease tuber and fibrous root, separate tuber and fibrous root, the air-dry surface moisture of room temperature after clear water is cleaned; Tuber and fibrous root are packed in the refrigerating plant ,-45 ℃ lower freezing, freeze 4h; Lepidinm meyenii Walp tuber after freezing is cut into the thick thin slice of 3mm, sends into-22 ℃ of Cold storage in the refrigerators with fibrous root; Lepidinm meyenii Walp tuber and fibrous root uniform spreading through cold preservation are loaded in the lyophilizing dish, after-45 ℃ pre-freeze, pack in the radiant heating type freeze drying plant, be evacuated to 55Pa, plait point-18 is set ℃ carries out sublimation drying, again with the parsing-desiccation of 45 ℃ of material central temperatures, until moisture content 2% obtains the dried active pueraria root powder; Sieve through Ordinary pulverization and through 250 eye mesh screens and to obtain the dried active pueraria root powder.Get the dry pueraria root powder that makes, measure glucosinolate content in the dried active Lepidinm meyenii Walp by the tablets by HPLC-MS among the agricultural industry criteria NY/T1103.3-2006 of the People's Republic of China (PRC), measurement result is: glucosinolate accounts for 1.43% of dry pueraria root powder gross weight.
Embodiment 7
The adjuvant (methylcellulose) of getting the dried active pueraria root powder adding pharmaceutical field acceptance of embodiment 1 preparation is prepared into tablet.
Embodiment 8
The dried active pueraria root powder of getting embodiment 2 preparations adds the adjuvant (dextrin) that pharmaceutical field is accepted, and is prepared into electuary after the pelletize.
Embodiment 9
The dried active pueraria root powder of getting embodiment 3 preparations does not add adjuvant and directly is prepared into capsule.
Embodiment 10
Get the ripe fresh Lepidinm meyenii Walp tuber of yellow, purple, black of Lijiang, yunnan non-polluted planting, under identical conditions, adopt respectively nature monoblock drying, natural chip drying, low-temperature vacuum drying and vacuum freeze-drying technique, the dry Lepidinm meyenii Walp goods that obtain adopt the tablets by HPLC-MS among the NY/T1103.3-2006 to measure glucosinolate content, result such as table 1:
The nature monoblock is dry: clean after the results, whole tuber carries out natural drying;
The nature chip drying: purge block undercut sheet after the results, carry out natural drying again;
Low-temperature vacuum drying: vacuum-0.075Mpa, 48 ~ 55 ℃ of temperature;
The condition of vacuum lyophilization such as embodiment 3
Table 1 Lepidinm meyenii Walp tuber adopts its active constituent content contrast of different drying modes
Embodiment 11
Get the dried active pueraria root powder A(tuber superfine powder of embodiment 5 preparations) and dried active pueraria root powder B(fibrous root superfine powder), with commercially available pueraria root powder, all adopt the tablets by HPLC-MS among the NY/T1103.3-2006 to measure glucosinolate content, as follows:
The dry pueraria root powder of table 2 embodiment 5 preparations and the total glucosinolate content of commercially available pueraria root powder are relatively
Dry pueraria root powder |
Total glucosinolate (g/100g) |
Dried active pueraria root powder B |
2.7 |
Dried active pueraria root powder A |
1.380 |
Pueraria root powder is produced in commercially available Xinjiang |
0.433 |
Commercially available Lijing produces pueraria root powder |
0.416 |
Commercially available Peru produces pueraria root powder |
0.107 |
Commercially available domestic Lepidinm meyenii Walp extract |
0.033 |
It is high that the present invention has total glucosinolate content, and nutrient substance keeps intact, the characteristics of nonirritant bad smell.