CN102432480B - Method for extracting lycine from Chinese wolfberry leaves - Google Patents
Method for extracting lycine from Chinese wolfberry leaves Download PDFInfo
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- CN102432480B CN102432480B CN201110364851.0A CN201110364851A CN102432480B CN 102432480 B CN102432480 B CN 102432480B CN 201110364851 A CN201110364851 A CN 201110364851A CN 102432480 B CN102432480 B CN 102432480B
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Abstract
The invention relates to a method for extracting lycine from Chinese wolfberry leaves. The method comprises the following steps of: (1) manually sorting Chinese wolfberry leaves, removing impurities, and drying in the shade indoors to obtain a dry Chinese wolfberry leaf sample; (2) smashing the dry Chinese wolfberry leaf sample, and sieving to obtain Chinese wolfberry leaf powder; (3) mixing the Chinese wolfberry leaf powder with water and leaching to obtain a leaching solution; (4) centrifugally separating the leaching solution to obtain a supernatant and filter residues; (5) adsorbing a filtrate with semi-polar macroporous adsorption resin, eluting with deionized water till sugar is removed completely, and eluting Chinese wolfberry leaf lycine adsorbed on the macroporous resin with a methanol-water-acetic acid solution to obtain an eluent containing Chinese wolfberry leaf lycine; and (6) concentrating the eluent containing Chinese wolfberry leaf lycine in vacuum under reduced pressure to obtain a Chinese wolfberry leaf lycine concentrated solution, and drying the Chinese wolfberry leaf lycine concentrated solution to obtain Chinese wolfberry leaf lycine powder. The method has low cost and high extracting rate.
Description
Technical field
The present invention relates to a kind of extraction preparation method of trimethyl-glycine, relate in particular to a kind of extracting method of Leaf of Matrimonyvine trimethyl-glycine.
Background technology
Leaf of Matrimonyvine is the leaf of Solanaceae (solanaceae) Lycium (Lycium Linn.) plant lycium barbarum (Lycium barbarum L.), is commonly called as a day essence grass, is light green, nontoxic, smell bitter cold.< < Compendium of Materia Medica > > points out, day smart grass energy " relieving restlessness benefit will, mends five kinds of strain and seven kinds of impairment, and high aspiration gas, removes the peel wind between skin joint, and the heat that disappears is malicious, and loose sore is swollen ".Leaf of Matrimonyvine is rich in trimethyl-glycine and the acid of multiple nitrogen base and trace element etc.In recent years pharmacology and clinical study show, trimethyl-glycine has strengthening immunity, reducing blood-fat, anti-oxidant, antitumor, promotes the multiple pharmacological effect such as metabolism of fat, anti-fatty liveranti-fatty liver, protection kidney, step-down, mitigation stress, improve a poor appetite, stable vitamin.
At present, the extraction preparation of trimethyl-glycine is adopted to pickling process, ultrasonic extraction conventionally.Wherein:
Pickling process is a kind of traditional natural product extraction method, and this method refers to that at ambient temperature the raw material crushing being put into the encloses container that fills appropriate solvent soaks with the stripping method of chemical composition wherein.The method operating process is quite time-consuming, and extraction efficiency is poor, several hours at least, needs at most time several weeks.Will reach dipping extraction needs to consume a large amount of solvents simultaneously completely, also can cause the potential loss of extracted compound and raw material, if at room temperature solvability is very poor as some compound, can not effectively be extracted.In addition, vat liquor easily goes mouldy, and need add appropriate sanitas as toluene, formaldehyde or chloroform etc.
Ultrasonic extraction is the method that adopts ultrasonic-assisted extraction solvent to extract.Mainly utilize hyperacoustic cavatition, destroy vegetable drug cell, make solvent be easy to infiltrate in cell, simultaneously due to hyperacoustic judder energy, strengthened release, diffusion and the dissolving of intracellular organic matter, accelerate the leaching of effective constituent.The method is extracted difficult control of temperature, and the thickness of wall of container and placement location are had relatively high expectations, and still for laboratory, uses on a small scale at present, and scale operation needs to solve plant issue.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of extracting method of with low cost, Leaf of Matrimonyvine trimethyl-glycine that extraction yield is high.
For addressing the above problem, the extracting method of a kind of Leaf of Matrimonyvine trimethyl-glycine of the present invention, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample;
(2) by described Leaf of Matrimonyvine dry sample after crushed, cross 20～320 mesh sieves, obtain Leaf of Matrimonyvine powder;
(3) described Leaf of Matrimonyvine powder and water are mixed by 1: 5～100 feed liquid mass volume ratio, after 10～40 ℃ of lixiviate 0.5～360h, obtain vat liquor;
(4) described vat liquor, through centrifugation, obtains supernatant liquor and filter residue;
(5) described filtrate is after intermediate-polarity macroporous adsorption resin absorption, first with deionized water, be eluted to sugar-free, with methanol-water-acetum wash-out of 2～50 times of bed volume, be adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin again, obtain the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine; Volume ratio in described methanol-water-acetum between methyl alcohol, water, acetic acid three is 5～10: 0.1～5: 0.01～3;
(6) by the described elutriant that contains Leaf of Matrimonyvine trimethyl-glycine after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution after drying, obtains Leaf of Matrimonyvine trimethyl-glycine powder.
By following preparation method, replace step described in claim 1 (3) to prepare vat liquor: described Leaf of Matrimonyvine powder and water are mixed by 1: 5～100 feed liquid mass volume ratio, at 50～100 ℃ of temperature, carry out heating in water bath, after refluxing extraction 0.5～72h, filter and get final product.
By following preparation method, replace step described in claim 1 (3) to prepare vat liquor: the ethanol that is 5～100% with mass concentration by described Leaf of Matrimonyvine powder mixes by 1: 5～100 feed liquid mass volume ratio, at 10～100 ℃ of temperature, carry out supersound extraction, after 0.1～72h, filter and get final product.
By following preparation method, replace step described in claim 1 (3) to prepare vat liquor: described Leaf of Matrimonyvine powder and water are mixed by 1: 5～100 feed liquid mass volume ratio, under the condition that is 20w～800w at power, carry out microwave extraction, after 0.1～5h, filter and get final product.
In described step (6), the condition of vacuum-concentrcted refers to that vacuum tightness is 0.03～0.07MPa, and temperature is 20～65 ℃.
In described step (6), drying temperature is 40～105 ℃.
The present invention compared with prior art has the following advantages:
1, because the present invention adopts the Leaf of Matrimonyvine that stock number is abundant, be raw material, therefore, effectively reduced production cost.
2, because leaching process Instrumental of the present invention operation of equipment is easy, technical parameter is easy to control, and therefore, can effectively improve extraction efficiency, is easy to large-scale industrialization and produces, and forms product product chain.
3, the Leaf of Matrimonyvine trimethyl-glycine extract of gained of the present invention is chocolate brown powder, pleasantly sweet, and yield >=20% detects through high performance liquid chromatography, wherein beet alkali content >=10%.
Embodiment
The extracting method of 1 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 4kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 40 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 10, after 10 ℃ of lixiviate 10h, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 4000r/min to vat liquor centrifugation 5min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 2 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 6: 2: 1.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.03MPa, temperature be under the condition of 30 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 40 ℃ of temperature, obtains 1.15kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 11.2%.
The extracting method of 2 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 50kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 20 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 25, after 40 ℃ of lixiviate 240h, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 3000r/min to vat liquor centrifugation 10min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 15 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 5: 5: 0.01.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.05MPa, temperature be under the condition of 20 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 65 ℃ of temperature, obtains 10.5kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 12.8%.
The extracting method of 3 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 10kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 320 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 100, after 20 ℃ of lixiviate 0.5h, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 5000r/min to vat liquor centrifugation 7min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 2 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 10: 0.1: 3.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.07MPa, temperature be under the condition of 65 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 105 ℃ of temperature, obtains 2.25kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 10.2%.
The extracting method of 4 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 3kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 80 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 5, after 30 ℃ of lixiviate 360h, obtain vat liquor.
(4) adopt whizzer with the centrifugal speed vat liquor centrifugation 12min of 2000r/min, obtain supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 50 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 9: 3: 1.5.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.06MPa, temperature be under the condition of 60 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 80 ℃ of temperature, obtains 0.66kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 11.2%.
The extracting method of 5 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 7kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 80 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 5, at 80 ℃ of temperature, carry out heating in water bath, after refluxing extraction 0.5h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 3200r/min to vat liquor centrifugation 10min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 5 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 9: 3: 2.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.04MPa, temperature be under the condition of 20 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 55 ℃ of temperature, obtains 1.44kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 12.2%.
The extracting method of 6 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 12kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 20 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 100, at 100 ℃ of temperature, carry out heating in water bath, after refluxing extraction 50h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 3400r/min to vat liquor centrifugation 8min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 2 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 5: 5: 3.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.03MPa, temperature be under the condition of 30 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 95 ℃ of temperature, obtains 2.68kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 14.6%.
The extracting method of 7 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 15kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 320 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 35, at 50 ℃ of temperature, carry out heating in water bath, after refluxing extraction 72h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 3800r/min to vat liquor centrifugation 10min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 50 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 10: 0.1: 0.01.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.07MPa, temperature be under the condition of 65 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 100 ℃ of temperature, obtains 3.02kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 12.2%.
The extracting method of 8 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 7kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 40 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 50, at 90 ℃ of temperature, carry out heating in water bath, after refluxing extraction 10h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 4000r/min to vat liquor centrifugation 10min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 30 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 6: 2: 1.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.03MPa, temperature be under the condition of 40 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 45 ℃ of temperature, obtains 0.66kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 13.6%.
The extracting method of 9 one kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 0.3kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 20 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) ethanol that is 5% by Leaf of Matrimonyvine powder with mass concentration mixes by the feed liquid mass volume ratio (kg/L) of 1: 5, at 100 ℃ of temperature, carries out supersound extraction, after 0.1h, filters, and obtains vat liquor.
(4) employing whizzer, with the centrifugal speed of 4400r/min to vat liquor centrifugation 10min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 50 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 5: 2: 1.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.03MPa, temperature be under the condition of 40 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 60 ℃ of temperature, obtains 0.066kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 11.9%.
The extracting method of 10 1 kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 0.25kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 320 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) ethanol that is 100% by Leaf of Matrimonyvine powder with mass concentration mixes by the feed liquid mass volume ratio (kg/L) of 1: 100, at 10 ℃ of temperature, carries out supersound extraction, after 5h, filters, and obtains vat liquor.
(4) employing whizzer, with the centrifugal speed of 4800r/min to vat liquor centrifugation 5min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 20 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 10: 0.1: 0.01.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.03MPa, temperature be under the condition of 65 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 85 ℃ of temperature, obtains 0.057kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 13.4%.
The extracting method of 11 1 kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 0.45kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 40 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) ethanol that is 70% by Leaf of Matrimonyvine powder with mass concentration mixes by the feed liquid mass volume ratio (kg/L) of 1: 80, at 60 ℃ of temperature, carries out supersound extraction, after 72h, filters, and obtains vat liquor.
(4) employing whizzer, with the centrifugal speed of 5000r/min to vat liquor centrifugation 20min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 2 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 6: 5: 3.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.07MPa, temperature be under the condition of 20 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 70 ℃ of temperature, obtains 0.099kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 14.5%.
The extracting method of 12 1 kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 0.05kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 20 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 100, under the condition that is 20w at power, carry out microwave extraction, after 5h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 4200r/min to vat liquor centrifugation 15min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 20 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 10: 0.1: 0.01.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.03MPa, temperature be under the condition of 65 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 75 ℃ of temperature, obtains 0.014kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 12.3%.
The extracting method of 13 1 kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 0.16kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 40 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 5, under the condition that is 400w at power, carry out microwave extraction, after 0.1h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 4500r/min to vat liquor centrifugation 10min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 50 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 5: 5: 3.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.07MPa, temperature be under the condition of 20 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 50 ℃ of temperature, obtains 0.038kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 13.6%.
The extracting method of 14 1 kinds of Leaf of Matrimonyvine trimethyl-glycines of embodiment, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample.
(2) 0.2kg Leaf of Matrimonyvine dry sample is put into pulverizer and pulverize, after pulverizing, cross 320 mesh sieves, obtain Leaf of Matrimonyvine powder.
(3) Leaf of Matrimonyvine powder is mixed with the feed liquid mass volume ratio (kg/L) of water by 1: 10, under the condition that is 800w at power, carry out microwave extraction, after 1h, filter, obtain vat liquor.
(4) employing whizzer, with the centrifugal speed of 2000r/min to vat liquor centrifugation 20min, obtains supernatant liquor and filter residue.Collect supernatant liquor and discard filter residue.
(5) filtrate, after intermediate-polarity macroporous adsorption resin absorption, is first eluted to sugar-free with deionized water, then is adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin with methanol-water-acetum wash-out of 2 times of bed volume, obtains the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine.
Wherein: the volume ratio (ml/ml/ml) in methanol-water-acetum between methyl alcohol, water, acetic acid three is 6: 3: 1.5.
(6) by the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine vacuum tightness be 0.06MPa, temperature be under the condition of 30 ℃ after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution is dried to constant weight at 90 ℃ of temperature, obtains 0.047kg brown Leaf of Matrimonyvine trimethyl-glycine powder.
Through high performance liquid chromatography, detect, in this Leaf of Matrimonyvine trimethyl-glycine powder, beet alkali content is 14.6%.
Claims (5)
1. an extracting method for Leaf of Matrimonyvine trimethyl-glycine, comprises the following steps:
(1) by Leaf of Matrimonyvine through manually picking after removal of impurities, indoor drying in the shade, obtains Leaf of Matrimonyvine dry sample;
(2) by described Leaf of Matrimonyvine dry sample after crushed, cross 20～320 mesh sieves, obtain Leaf of Matrimonyvine powder;
(3) described Leaf of Matrimonyvine powder is mixed by the feed liquid mass volume ratio of 1:5～100 with water, under the condition that is 20w～800w at power, carry out microwave extraction, after 0.1～5h, filter and obtain vat liquor;
(4) described vat liquor, through centrifugation, obtains supernatant liquor and filter residue;
(5) described supernatant liquor is after intermediate-polarity macroporous adsorption resin absorption, first with deionized water, be eluted to sugar-free, with methanol-water-acetum wash-out of 2～50 times of bed volume, be adsorbed on the Leaf of Matrimonyvine trimethyl-glycine on macroporous resin again, obtain the elutriant that contains Leaf of Matrimonyvine trimethyl-glycine; Volume ratio in described methanol-water-acetum between methyl alcohol, water, acetic acid three is 5～10:0.1～5:0.01～3;
(6) by the described elutriant that contains Leaf of Matrimonyvine trimethyl-glycine after vacuum-concentrcted, obtain Leaf of Matrimonyvine trimethyl-glycine concentrated solution; This Leaf of Matrimonyvine trimethyl-glycine concentrated solution after drying, obtains Leaf of Matrimonyvine trimethyl-glycine powder.
2. the extracting method of a kind of Leaf of Matrimonyvine trimethyl-glycine as claimed in claim 1, it is characterized in that: by following preparation method, replace step described in claim 1 (3) to prepare vat liquor: described Leaf of Matrimonyvine powder is mixed by the feed liquid mass volume ratio of 1:5～100 with water, at 50～100 ℃ of temperature, carry out heating in water bath, after refluxing extraction 0.5～72h, filter and get final product.
3. the extracting method of a kind of Leaf of Matrimonyvine trimethyl-glycine as claimed in claim 1, it is characterized in that: by following preparation method, replace step described in claim 1 (3) to prepare vat liquor: the ethanol that is 5～100% with mass concentration by described Leaf of Matrimonyvine powder mixes by the feed liquid mass volume ratio of 1:5～100, at 10～100 ℃ of temperature, carry out supersound extraction, after 0.1～72h, filter and get final product.
4. the extracting method of a kind of Leaf of Matrimonyvine trimethyl-glycine as claimed in claim 1, is characterized in that: in described step (6), the condition of vacuum-concentrcted refers to that vacuum tightness is 0.03～0.07MPa, and temperature is 20～65 ℃.
5. the extracting method of a kind of Leaf of Matrimonyvine trimethyl-glycine as claimed in claim 1, is characterized in that: in described step (6), drying temperature is 40～105 ℃.
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| CN103549421B (en) * | 2013-10-24 | 2015-07-29 | 格尔木源鑫堂生物科技有限公司 | A kind of medlar multi-vitamins imitates fast powder and production method thereof |
| CN104839738B (en) * | 2015-04-27 | 2017-03-08 | 宁夏森淼种业生物工程有限公司 | A kind of method of supercritical ultrasonics technology high efficiency extraction folium lycii mineral element |
| CN104829474B (en) * | 2015-05-27 | 2017-02-01 | 中国科学院西北高原生物研究所 | Method for preparing glycine betaine chemical reference substances from boxthorn leaves |
| CN106177170A (en) * | 2016-07-30 | 2016-12-07 | 成都薇诺娜生物科技有限公司 | Fructus Lycii crop is used to extract the preparation method of Fructus Lycii flavone |
| CN106242986A (en) * | 2016-07-30 | 2016-12-21 | 成都薇诺娜生物科技有限公司 | Fructus Lycii root is used to extract the preparation method of glycine betaine |
| CN107266327A (en) * | 2017-06-25 | 2017-10-20 | 宜兴市天石饲料有限公司 | A kind of isolation and purification method of natural glycine betaine |
| CN107537845B (en) * | 2017-09-01 | 2021-03-16 | 贵州大学 | Method for controlling release of coal gangue pollutants |
| CN113698309B (en) * | 2021-09-10 | 2024-02-06 | 中南民族大学 | Method for extracting and separating betaine fat from bolete |
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