CN107501994A - A kind of method with microwave ultrasonic extraction purple highland barley pigment - Google Patents
A kind of method with microwave ultrasonic extraction purple highland barley pigment Download PDFInfo
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- CN107501994A CN107501994A CN201710946155.8A CN201710946155A CN107501994A CN 107501994 A CN107501994 A CN 107501994A CN 201710946155 A CN201710946155 A CN 201710946155A CN 107501994 A CN107501994 A CN 107501994A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Non-Alcoholic Beverages (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The invention discloses a kind of method with microwave ultrasonic extraction purple highland barley pigment, belong to nature strength technical field, the extracting method comprises the following steps：A. pretreatment of raw material：Select without insect bite, without the whole grain purple highland barley or purple highland barley powder gone mouldy, after removing debris, wash clean, drying process；B. extract：The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and adjust pH value after 0.5~2, after handling 30~60min, centrifugation, filtering, to take supernatant to obtain the pigment.The extracting method of the present invention has the advantages of recovery rate is high, and raw material availability is high and cost is low.
Description
Technical field
The present invention relates to a kind of method with microwave ultrasonic extraction purple highland barley pigment, belong to chemical technology field.
Background technology
Food colour is the important component of food additives, and synthetic dyestuff is so that its is bright in luster, stability is good, is easy to
The features such as coloring, was once widely used.But with the development of modern science, it has been found that synthetic food color is to people
Body has different degrees of toxicity even carcinogenicity, and natural pigment has the characteristics of safe and non-toxic, nutrition added valve is high, just increasingly
Favored by people.Therefore, various edible natural pigments are extracted and separated from natural products substitutes artificial synthesized color
Element is as one of focus of field of food science research.
Purple highland barley is the new varieties that the Lhasa institute of agricultural sciences comes out from common highland barley breed breeding in recent years, although mouthfeel and production
Amount is all not so good as white highland barley, but it is rich in the natural pigments such as anthocyanidin.Anthocyanidin has been used more as a kind of natural food colour
Year, side effect is found no so far, and with strong anti-oxidation, the function that resistance is different, antitumor.If can be in purple highland barley
Natural pigment carries out developmental research, can not only deepen the deep processing of purple this agricultural product of highland barley, more likely develop new
Health food.
Start to develop and utilize highland barley pigment, such as Publication No. CN102898863B, entitled " highland barley monascus
The patent of invention of the purposes of pigment and preparation method thereof and highland barley monascus pigment in food ", it is exactly one kind using highland barley
Fermented product extracts pigment, and patent extraction is monascorubin, it is impossible to extracts purple highland barley pigment using this method.Currently for
Also there is some new methods, new technology based on traditional water bath method in the extractive technique of highland barley anthocyanidin, but still
In the presence of the shortcomings of time-consuming, extraction is not thorough.And for example publication number CN1032776026, a kind of entitled " lactobacillus-fermented extraction
The patent of invention of the method for anthocyanin in highland barley " extracts anthocyanin by lactobacillus-fermented purple highland barley skin, although anthocyani pigment
Yield increased compared with conventional method, but this method only fermenting step just needs 3~4d, extraction time length, and efficiency is low；And for example
Publication number CN103288899A, the patent of invention of entitled " a kind of method that anthocyanin is separated from purple highland barley " first will be purple blue or green
Highland barley skin soaks 1~2h, next adds 2~3h of alcohol steep, then adds the materials such as glucose, acetic acid, natural flavone and enter
Row ultrasonic extraction anthocyanin, 4~6h, whole extracting cycle time length, complex steps are finally also soaked, and also need to add
The materials such as natural flavone, not only efficiency is low also add extraction cost.Therefore, in order to improve the added value of highland barley products, extend
The industrial chain of highland barley products, need a kind of simple, technology of high efficiency extraction purple highland barley pigment of exploitation badly.
The content of the invention
Present invention seek to address that the technical problem that pigment recovery rate is not high in the prior art, time-consuming, cost is high, there is provided one
The new method with microwave ultrasonic extraction purple highland barley pigment of kind, the method by the way that ultrasonic extraction and Microwave Extraction are combined, is carried
The recovery rate of high pigment, shorten extracting cycle, reduce extraction cost.
In order to realize foregoing invention purpose, technical scheme is as follows：
A kind of method with microwave ultrasonic extraction purple highland barley pigment, it is characterised in that：Comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley or purple highland barley powder gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in ultrasonic-microwave extractor, add extractant, and adjust pH value as 0.5
After~2, after extracting 30~60min, centrifugation, filtering, supernatant is taken to obtain the purple highland barley pigment.
Further, in step A, the raw material selects whole grain purple highland barley.
Further, in step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and through being sieved through remove it is small
Granule foreign.
Further, in step B, the extractant is one kind in ethanol, methanol, EtOH-EtOAc.
Further, in step B, the extractant is ethanol.
Further, in step B, the volumetric concentration of the ethanol is 40~60%.
Further, in step B, solid-liquid ratio is 1 in the extraction process:5~1：10.
Further, in step B, the Extracting temperature is 60~80 DEG C.
Further, in step B, the power of the microwave is 50~150W.
Further, in step B, the ultrasonic power is 200~500W.
Beneficial effects of the present invention：
（1）The present invention uses specific extracting parameter by the way that microwave and ultrasonic extraction mode are combined, and it is blue or green to improve purple
The recovery rate of pigment in highland barley, specifically, microwave provide the possibility for heating to solid particle indirect and selectively heating,
Cavitation caused by ultrasound can then provide a large amount of concentrate and release energy, and improve heating and energy when two kinds of technical tie-ups use
Respective advantage can be played during amount transfer, microwave-ultrasonic GC-MS is shown in the extraction of natural product active ingredient
Big advantage, can make full use of judder caused by ultrasonic wave, cavitation effect, stirring action and microwave reflection,
Penetrate, absorb, the features such as fuel factor and seepage velocity are fast, significantly improving the extracted amount of active component, shortening extraction time, simultaneously
Reduce solvent using, reduce environmental pollution.
（2）In the present invention, raw material selection whole grain purple highland barley, compared to purple highland barley powder, the extraction of whole grain purple highland barley
Rate is higher, because purple highland barley anthocyanidin is primarily present in the epidermis of highland barley, more starch is contained in purple highland barley, if
Highland barley is crushed, starch can be gelatinized at high temperature, and starch granules can be swelled, divide and form homogeneous paste solution, so as to form one
It is individual it is netted contain hydrocolloid, pigment molecular can be made viscid, be not easy to the complete extraction of pigment molecular.
（3）The extracting method obtained by the selection of extracting mode and the special parameter set according to method, may be such that purple
The extraction rate reached of pigment is to more than 40mg/g in color highland barley, significantly larger than using the recovery rate of the method in background technology.
Embodiment
The present invention is described in further detail with reference to embodiment, but the implementation of the present invention is not limited to this.
Embodiment 1
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the purple highland barley powder to go mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 2.0, it is placed in hot bath, after handling 30min simultaneously with microwave and ultrasound, centrifugation, filtering, takes supernatant to obtain described
Pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is the EtOH-EtOAc that volumetric concentration is 40%.
In step B, it is 1 to state solid-liquid ratio in extraction process:5.
In step B, the temperature of the extraction is 60 DEG C.
In step B, the power of the microwave is 50W.
In step B, the ultrasonic power is 300W.
Embodiment 2
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 1.5, it is placed in hot bath, after handling 40min simultaneously with microwave and ultrasound, centrifugation, filtering, takes supernatant to obtain described
Pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is the ethanol that volumetric concentration is 60%.
In step B, it is 1 to state solid-liquid ratio in extraction process:10.
In step B, the temperature of hot water is 70 DEG C in the hot bath.
In step B, the power of the microwave is 50W.
In step B, the ultrasonic power is 300W.
Embodiment 3
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 1.0, it is placed in hot bath, after handling 30min simultaneously with microwave and ultrasound, centrifugation, filtering, takes supernatant to obtain described
Pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is the methanol that volumetric concentration is 60%.
In step B, it is 1 to state solid-liquid ratio in extraction process:10.
In step B, the temperature of hot water is 70 DEG C in the hot bath.
In step B, the power of the microwave is 150W.
In step B, the ultrasonic power is 200W.
Embodiment 4
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 1.5, it is placed in hot bath, after handling 30min simultaneously with microwave and ultrasound, centrifugation, filtering, takes supernatant to obtain described
Pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is that volumetric concentration is 60% ethanol.
In step B, it is 1 to state solid-liquid ratio in extraction process:10.
In step B, the temperature of hot water is 80 DEG C in the hot bath.
In step B, the power of the microwave is 50W.
In step B, the ultrasonic power is 300W.
Embodiment 5
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 0.5, it is placed in hot bath, after handling 40min simultaneously with microwave and ultrasound, centrifugation, filtering, takes supernatant to obtain described
Pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is the ethanol that volumetric concentration is 60%.
In step B, it is 1 to state solid-liquid ratio in extraction process: 10.
In step B, the temperature of hot water is 70 DEG C in the hot bath.
In step B, the power of the microwave is 50W.
In step B, the ultrasonic power is 300W.
Embodiment 6
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 1.5, it is placed in hot bath, after 30min is ultrasonically treated, centrifugation, filtering, takes supernatant to obtain the pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is the ethanol that volumetric concentration is 60%.
In step B, it is 1 to state solid-liquid ratio in extraction process: 10.
In step B, the temperature of hot water is 70 DEG C in the hot bath.
In step B, the ultrasonic power is 500W.
Microwave ultrasound extractor in the present embodiment uses microwave ultrasonic wave Chinese medicine extraction machine of the prior art, model
XO-SM200。
Embodiment 7
A kind of method with microwave ultrasonic extraction purple highland barley pigment, comprise the following steps：
A. pretreatment of raw material
Select without insect bite, without the whole grain purple highland barley gone mouldy, after removing debris, wash clean, drying process；
B. extract
The pretreated purple highland barleys of step A are placed in microwave ultrasound extractor, add extractant, and with salt acid for adjusting pH value
After 1.5, it is placed in hot bath, after microwave treatment 30min, centrifugation, filtering, takes supernatant to obtain the pigment.
In step A, the removal of impurities refers to remove the small debris of proportion with selection by winnowing, and removes little particle impurity by being sieved through.
In step B, the extractant is the ethanol that volumetric concentration is 60%.
In step B, it is 1 to state solid-liquid ratio in extraction process: 10.
In step B, the temperature of hot water is 70 DEG C in the hot bath.
In step B, the power of the microwave is 150W.
It please provide above-described embodiment 1 ~ 5（The present invention）And embodiment 6,7（Using the control group of single extracting mode）Carry
Pigment is taken, the recovery rate correction data being calculated.
Table 1：
By contrast, pigment is extracted by the way of ultrasound in the present invention and microwave combine, by diluting and keeping away
Light measurement absorbance A, the recovery rate being calculated relatively use single method（Embodiment 6,7）Recovery rate it is high.
It should be noted that the computational methods of recovery rate are as follows：
Obtained supernatant dilution and lucifuge measure absorbance A will be extracted, so as to calculate recovery rate, calculation formula is as follows：
In formula, pigment recovery rate,（mg/g）；A530For the absorbance under 530 nm, V is the volume after dilution, mL；N is dilution
Multiple；98.2 be the average extinction coefficient of anthocyanidin；M is example weight, g.
It is described above, be only presently preferred embodiments of the present invention, any formal limitation not done to the present invention, it is every according to
Any simply modification, the equivalent variations made according to the technical spirit of the present invention to above example, each fall within the protection of the present invention
Within the scope of.
Claims (10)
- A kind of 1. method with microwave ultrasonic extraction purple highland barley pigment, it is characterised in that：Comprise the following steps：Pretreatment of raw materialSelect without insect bite, without the whole grain purple highland barley or purple highland barley powder gone mouldy, after removing debris, wash clean, drying process；B. extractThe pretreated purple highland barleys of step A are placed in ultrasonic-microwave extractor, add extractant, and adjust pH value as 0.5 After~2, after extracting 30~60min, centrifugation, filtering, supernatant is taken to obtain the purple highland barley pigment.
- 2. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 1, it is characterised in that：In step A, institute State raw material selection whole grain purple highland barley.
- 3. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 1, it is characterised in that：In step A, institute State removal of impurities to refer to remove the small debris of proportion with selection by winnowing, and little particle impurity is removed by being sieved through.
- 4. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 1, it is characterised in that：In step B, institute Extractant is stated as one kind in ethanol, methanol, EtOH-EtOAc.
- 5. the method for pigment is extracted from purple highland barley as claimed in claim 1, it is characterised in that：In step B, the extraction Agent is ethanol.
- 6. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 5, it is characterised in that：In step B, institute The volumetric concentration for stating ethanol is 40~60%.
- 7. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 1, it is characterised in that：In step B, institute It is 1 to state solid-liquid ratio in extraction process:5~1：10.
- 8. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 1, it is characterised in that：In step B, institute Extracting temperature is stated as 60~80 DEG C.
- 9. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 1, it is characterised in that：In step B, institute The power for stating microwave is 50~150W.
- 10. the method for microwave ultrasonic extraction purple highland barley pigment is used as claimed in claim 9, it is characterised in that：In step B, The ultrasonic power is 200~500W.
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| CN201710946155.8A CN107501994A (en) | 2017-10-12 | 2017-10-12 | A kind of method with microwave ultrasonic extraction purple highland barley pigment |
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| CN201710946155.8A CN107501994A (en) | 2017-10-12 | 2017-10-12 | A kind of method with microwave ultrasonic extraction purple highland barley pigment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111317136A (en) * | 2020-03-17 | 2020-06-23 | 中国科学院西北高原生物研究所 | Preparation method and application of highland barley product |
| CN111631294A (en) * | 2020-06-08 | 2020-09-08 | 陕西科技大学 | Purple highland barley anthocyanin-rich soft sweet and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288899A (en) * | 2013-05-24 | 2013-09-11 | 西藏月王生物技术有限公司 | Method of separating anthocyanin from purple highland barley |
-
2017
- 2017-10-12 CN CN201710946155.8A patent/CN107501994A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288899A (en) * | 2013-05-24 | 2013-09-11 | 西藏月王生物技术有限公司 | Method of separating anthocyanin from purple highland barley |
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| 张文会 等: "超声波提取青稞黄酮类化合物工艺研究", 《农产品加工》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111317136A (en) * | 2020-03-17 | 2020-06-23 | 中国科学院西北高原生物研究所 | Preparation method and application of highland barley product |
| CN111631294A (en) * | 2020-06-08 | 2020-09-08 | 陕西科技大学 | Purple highland barley anthocyanin-rich soft sweet and preparation method thereof |
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