CN104839738B - A kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element - Google Patents
A kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element Download PDFInfo
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- CN104839738B CN104839738B CN201510204263.9A CN201510204263A CN104839738B CN 104839738 B CN104839738 B CN 104839738B CN 201510204263 A CN201510204263 A CN 201510204263A CN 104839738 B CN104839738 B CN 104839738B
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- 238000000605 extraction Methods 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002366 mineral element Substances 0.000 title claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 47
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229960000583 acetic acid Drugs 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 23
- 239000000284 extract Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims abstract description 3
- 238000005238 degreasing Methods 0.000 claims abstract description 3
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 3
- 239000006228 supernatant Substances 0.000 claims description 62
- 238000000967 suction filtration Methods 0.000 claims description 43
- 238000002390 rotary evaporation Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 24
- 238000001556 precipitation Methods 0.000 claims description 22
- 238000002525 ultrasonication Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 238000002137 ultrasound extraction Methods 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 44
- 239000000706 filtrate Substances 0.000 description 40
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 22
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 22
- 239000011575 calcium Substances 0.000 description 22
- 229910052791 calcium Inorganic materials 0.000 description 22
- 229910052742 iron Inorganic materials 0.000 description 22
- 229910052725 zinc Inorganic materials 0.000 description 22
- 239000011701 zinc Substances 0.000 description 22
- 241000037488 Coccoloba pubescens Species 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- 244000046052 Phaseolus vulgaris Species 0.000 description 20
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 20
- 238000005119 centrifugation Methods 0.000 description 20
- 239000012065 filter cake Substances 0.000 description 20
- 238000004519 manufacturing process Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 244000241838 Lycium barbarum Species 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 244000241872 Lycium chinense Species 0.000 description 1
- 235000015468 Lycium chinense Nutrition 0.000 description 1
- 235000017784 Mespilus germanica Nutrition 0.000 description 1
- 244000182216 Mimusops elengi Species 0.000 description 1
- 235000000560 Mimusops elengi Nutrition 0.000 description 1
- 235000007837 Vangueria infausta Nutrition 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 230000002232 neuromuscular Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 108010048734 sclerotin Proteins 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000005418 vegetable material Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Medicines Containing Plant Substances (AREA)
- Peptides Or Proteins (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element.It is characterized in, comprises the steps：(1) raw material：Folium lycii is dried；(2) crush：Folium lycii after drying is crushed；(3) sieve：Folium lycii powder after crushing is crossed 30 100 mesh sieves；(4) degreasing；(5) it is acidified：Add the deionized water of 20 60 times of folium lycii powder volume, and add material liquid volume 1/2 1/10 glacial acetic acid, stand 1.5 2h；(6) ultrasonic wave extraction；(7) filter；(8) concentrate：Reduced pressure concentration is carried out to the 1/3 1/5 of original volume to the extract for obtaining with vacuum distillation apparatus；(9) dry：Dry, obtain final product.The ultrasonic extraction that the present invention is adopted is a kind of method of high efficiency extraction folium lycii mineral element, with time-consuming short, mineral element yield high, mineral element destructiveness is little, save material and the low advantage of operating cost.
Description
Technical field
The present invention relates to a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element.
Background technology
Folium lycii (Foliis medlar) is referred to as " day essence grass ", cool in nature, quenches one's thirst and promotes the production of body fluid, and yin-nourishing is relieved inflammation or internal heat, rich in multiple micro-
Secondary element, its Mineral Elements Content are even more than Chinese wolfberry fruit.Mineral element plays the role of much important, human body shortage to human body
When, disease can be produced.Calcium, iron, zinc are all trace elements needed by human.Calcium can promote bone and sclerotin strong, or Neuromuscular
The requisite material such as meat；Iron is the requisite material of synthetic hemoglobin, and shortage can cause anaemia；The shortage of zinc can be led
Cause depauperation, withered and yellowish hairs, dispersion attention etc..People are mainly from food some mineral units necessary to intake body
Element.The extracting method of plant Mineral Elements is only limitted to ashing method and nitrification process, and the purpose of extraction is intended merely to detect its content,
After extraction, these mineral elements have been out edibility, in these processes to the extraction of mineral element element be destroy
Property.One kind is not all found in current either these retrieval or patent retrieval can be efficiently and non-destructively from plant
A large amount of effective ways for extracting mineral element.
Content of the invention
It is an object of the invention to provide a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element, effectively can carry
The yield of high mineral element, so as to economizing in raw materials, reducing production cost.
A kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element, which is particular in that, comprises the steps：
(1) raw material：Folium lycii is dried；
(2) crush：Folium lycii after drying is crushed；
(3) sieve：Folium lycii powder after crushing is crossed 30-100 mesh sieve；
(4) degreasing：No. 6 light petrols are added in powder and make No. 6 light petrol liquid levels not have powder 1-1.5cm, stirring,
Suction filtration, dries 1-3h in 40-60 DEG C of drying under reduced pressure case, obtains removing the folium lycii powder of fat；
(5) it is acidified：Folium lycii powder is taken, the deionized water of folium lycii powder volume 20-60 times is added, and adds feed liquid
The glacial acetic acid of the 1/2-1/10 of volume, stands 1.5-2h；
(6) ultrasonic wave extraction：At 30-100 DEG C, ultrasonic wave extraction 5min-60min under the conditions of 50-100MHz, take ultrasonic wave
Supernatant after process, remaining precipitation is extracted 2-4 time again according to above-mentioned supersonic extracting method, merges all extracts；
(7) filter：By extract suction filtration, filter residue is discarded；
(8) concentrate：Reduced pressure concentration is carried out to the 1/3-1/5 of original volume to the extract for obtaining with vacuum distillation apparatus；
(9) dry：Dry, that is, obtain mineral element extract.
The method that reduced pressure concentration is adopted in step (8) is rotary evaporation, and the temperature of rotary evaporation is 20-80 DEG C, and rotation is steamed
The final volume that sends out is the 1/2-1/6 of original solution volume.
In step (1) specifically by folium lycii in the blast drier 50-60 DEG C of drying 8-12h.
Crush in step (2) and specifically adopt medicinal herb grinder.
In step (4), stirring specifically adopts magnetic stirrer 20-30min.
Dry in step (6) and specifically refer to the liquid after concentration is Tumblied Dry at 50-60 DEG C.
The inventive method is with respect to the advantage of prior art：
(1) for the first time provide a kind of efficient and nondestructive extract mineral element method, utilize be in acidolysis
On the basis of, add the condition of ultrasonic wave extraction so that dissolution rate and dissolution rate of the mineral element from matrimony vine leaf cell are all
Increase, raw material and the purpose of time is saved so as to reach.
(2) ultrasonic wave is the friendship frequency signal sent using supersonic generator, and it is frequently mechanical to be struck a bargain by transducer conversion
Shake and travel in cleaning fluid, " cavitation " phenomenon is produced, i.e., in cleaning fluid in the form of " bubble ", produce fracture phenomena.
Ultrasonic wave has efficient, economy, low cost, saves the cost brought because of labour.
(3) extraction efficiency of ultrasonic wave extraction folium lycii Mineral Elements is very high, can once extract multiple minerals unit
Element, and a large amount of extractions of mineral element can be carried out.
(4) extracting the mineral element for obtaining by the use of ultrasonic extraction from vegetable material can be used as edible nutrition
Replenishers or food additives are used for food processing.
(5) as the equipment used by this method is relatively simple, pulverizer, ultrasonic device, vavuum pump and vacuum have simply been used
Drying equipment, therefore its operating cost is relatively low, is more suitable for industrialized production.
In sum, the ultrasonic extraction that the present invention is adopted is a kind of method of high efficiency extraction folium lycii mineral element,
Have that time-consuming short, mineral element yield is high, mineral element destructiveness is little, save material and the low advantage of operating cost, more
Be conducive to industrialized production and the consecutive production in modern times.
Specific embodiment
The inventive method creatively make use of the work characteristics that ultrasonic cavitation extraction is acted on, and non-destructively carry first
Contained mineral element is taken in folium lycii, can make the mineral element of extraction can be strong as nutrient health replenishers or food
Agent.
Numbering in table 1 below corresponds to following embodiments.
Table 1：Mineral element extracted amount under different condition：
Embodiment 1：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 30 DEG C, ultrasonic wave extraction 5min under 50MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant carries out rotary evaporation to the 1/5 of original volume.
6. the liquid after concentration is dried, the content for obtaining calcium is 1.4021mg/g, and the content of iron is 0.0023mg/g, zinc
Content be 0.0071mg/g.
Embodiment 2：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 30 DEG C, ultrasonic wave extraction 10min under 50MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4273mg/g, and the content of iron is 0.0027mg/g, the containing of zinc
Amount is 0.0073mg/g.
Embodiment 3：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 30 DEG C, ultrasonic wave extraction 15min under 50MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4032mg/g, and the content of iron is 0.0025mg/g, the containing of zinc
Amount is 0.0073mg/g.
Embodiment 4：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 30 DEG C, ultrasonic wave extraction 20min under 50MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4005mg/g, and the content of iron is 0.0026mg/g, the containing of zinc
Amount is 0.0074mg/g.
Embodiment 5：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 30 DEG C, ultrasonic wave extraction 25min under 50MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.3982mg/g, and the content of iron is 0.0031mg/g, the containing of zinc
Amount is 0.0072mg/g.
Embodiment 6：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 5min under 80MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.5526mg/g, and the content of iron is 0.0025mg/g, the containing of zinc
Amount is 0.0076mg/g.
Embodiment 7：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 10min under 80MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.5619mg/g, and the content of iron is 0.0031mg/g, the containing of zinc
Amount is 0.0079mg/g.
Embodiment 8：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 15min under 80MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.5288mg/g, and the content of iron is 0.0031mg/g, the containing of zinc
Amount is 0.0077mg/g.
Embodiment 9：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 20min under 80MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.5273mg/g, and the content of iron is 0.0029mg/g, the containing of zinc
Amount is 0.0076mg/g.
Embodiment 10：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 25min under 80MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.5247mg/g, and the content of iron is 0.0028mg/g, the containing of zinc
Amount is 0.0075mg/g.
Embodiment 11：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 5min under 100MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4755mg/g, and the content of iron is 0.0023mg/g, the containing of zinc
Amount is 0.0068mg/g.
Embodiment 12：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 10min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.5012mg/g, and the content of iron is 0.0026mg/g, the containing of zinc
Amount is 0.0071mg/g.
Embodiment 13：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 15min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4904mg/g, and the content of iron is 0.0029mg/g, the containing of zinc
Amount is 0.0070mg/g.
Embodiment 14：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 20min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4786mg/g, and the content of iron is 0.0028mg/g, the containing of zinc
Amount is 0.0066mg/g.
Embodiment 15：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 50 DEG C, ultrasonic wave extraction 25min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4273mg/g, and the content of iron is 0.0027mg/g, the containing of zinc
Amount is 0.0068m g/g.
Embodiment 16：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 70 DEG C, ultrasonic wave extraction 5min under 100MHz, take the supernatant after ultrasonication, by remaining precipitation according to
Above-mentioned supersonic extracting method is extracted twice again, and the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4279mg/g, and the content of iron is 0.0029mg/g, the containing of zinc
Amount is 0.0066mg/g.
Embodiment 17：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 70 DEG C, ultrasonic wave extraction 10min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4282mg/g, and the content of iron is 0.0028mg/g, the containing of zinc
Amount is 0.0067mg/g.
Embodiment 18：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 70 DEG C, ultrasonic wave extraction 15min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4525mg/g, and the content of iron is 0.0031mg/g, the containing of zinc
Amount is 0.0066mg/g.
Embodiment 19：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 70 DEG C, ultrasonic wave extraction 20min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate constant volume to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4426mg/g, and the content of iron is 0.0034mg/g, the containing of zinc
Amount is 0.0065mg/g.
Embodiment 20：
1. folium lycii (folium lycii is from large-leaf fructus lycii healthcare Qi of the 2 years age of trees in Beijing bean sprout base) is cleaned, dry at 60 DEG C
12h, grinds and crosses 60 mesh sieves.
2. powder that 1g sieves accurately is weighed in beaker, add suction filtration after No. 6 light petrol 6mL stirring 20min.
3. filter cake is moved into the deionized water that 10mL is added in beaker, adds the glacial acetic acid that 2mL concentration is 50%, standing two
Individual hour.
4. at 70 DEG C, ultrasonic wave extraction 25min under 100MHz, the supernatant after ultrasonication is taken, remaining precipitation is pressed
Extract again twice according to above-mentioned supersonic extracting method, the liquid of three ultrasonic wave extractions is merged suction filtration, filtrate (uses deionization
Water) constant volume is to 50mL.
5. 200mL absolute ethyl alcohol is added in the good filtrate of constant volume, and standing 2h is fully precipitated, and centrifugation obtains supernatant, will
Supernatant rotary evaporation is to the 1/5 of original volume.
6. the liquid after concentration is dried, the content of calcium is 1.4482mg/g, and the content of iron is 0.0032mg/g, the containing of zinc
Amount is 0.0067mg/g.
Claims (6)
1. a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element, it is characterised in that comprise the steps：
（1）Raw material：Folium lycii is dried；
（2）Crush：Folium lycii after drying is crushed；
（3）Screening：Folium lycii powder after crushing is crossed 30-100 mesh sieve；
（4）Degreasing：No. 6 light petrols are added in powder and make No. 6 light petrol liquid levels not have powder 1-1.5cm, stirring, take out
Filter, dries 1-3h in 40-60 DEG C of drying under reduced pressure case, obtains removing the folium lycii powder of fat；
（5）Acidifying：Folium lycii powder is taken, the deionized water of folium lycii powder volume 20-60 times is added, and adds material liquid volume
1/2-1/10 glacial acetic acid, stand 1.5-2h；
（6）Ultrasonic wave extraction：At 30-100 DEG C, ultrasonic wave extraction 5min-60min under the conditions of 50-100MHz, take ultrasonication
Supernatant afterwards, remaining precipitation is extracted 2-4 time again according to above-mentioned supersonic extracting method, merges all extracts；
（7）Filter：By extract suction filtration, filter residue is discarded；
（8）Concentrate：Reduced pressure concentration is carried out to the 1/3-1/5 of original volume to the extract for obtaining with vacuum distillation apparatus；
（9）Dry：Dry, that is, obtain mineral element extract.
2. a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element as claimed in claim 1, it is characterised in that：Step
Suddenly（8）The method that middle reduced pressure concentration is adopted is rotary evaporation, and the temperature of rotary evaporation is 20-80 DEG C, the final body of rotary evaporation
Product is the 1/2-1/6 of original solution volume.
3. a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element as claimed in claim 1, it is characterised in that：Step
Suddenly（1）In specifically by folium lycii in the blast drier 50-60 DEG C of drying 8-12h.
4. a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element as claimed in claim 1, it is characterised in that：Step
Suddenly（2）Middle crushing specifically adopts medicinal herb grinder.
5. a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element as claimed in claim 1, it is characterised in that：Step
Suddenly（4）Middle stirring specifically adopts magnetic stirrer 20-30 min.
6. a kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element as claimed in claim 1, it is characterised in that：Step
Suddenly（9）Middle drying specifically refers to the liquid after concentration is Tumblied Dry at 50-60 DEG C.
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Address after: Victory Street Xingqing District of Yinchuan City No. 1059 the Ningxia Hui Autonomous Region 750004 Patentee after: Senmiao Technology Group Limited by Share Ltd Address before: Victory Street Xingqing District of Yinchuan City No. 1059 the Ningxia Hui Autonomous Region 750004 Patentee before: Ningxia Senmiao Seed Industry Biological Engineering Co., Ltd. |
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