CN102796207B - Method for extracting pectin from tangerine peel - Google Patents
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- 239000001814 pectin Substances 0.000 title claims abstract description 33
- 229920001277 pectin Polymers 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 28
- 241000675108 Citrus tangerina Species 0.000 title abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000000341 volatile oil Substances 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000284 extract Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
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- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
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- 238000001914 filtration Methods 0.000 claims description 4
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- 239000003002 pH adjusting agent Substances 0.000 claims description 4
- 238000002390 rotary evaporation Methods 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
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- 238000000605 extraction Methods 0.000 abstract description 6
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- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 235000019198 oils Nutrition 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
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- XMGQYMWWDOXHJM-JTQLQIEISA-N (+)-α-limonene Chemical compound CC(=C)[C@@H]1CCC(C)=CC1 XMGQYMWWDOXHJM-JTQLQIEISA-N 0.000 description 2
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 2
- 241000207199 Citrus Species 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- MOYAFQVGZZPNRA-UHFFFAOYSA-N Terpinolene Chemical compound CC(C)=C1CCC(C)=CC1 MOYAFQVGZZPNRA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- UAHWPYUMFXYFJY-UHFFFAOYSA-N beta-myrcene Chemical compound CC(C)=CCCC(=C)C=C UAHWPYUMFXYFJY-UHFFFAOYSA-N 0.000 description 2
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- 235000020971 citrus fruits Nutrition 0.000 description 2
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- GJYKUZUTZNTBEC-IVZWLZJFSA-N (1R,4S,5R)-4-methyl-1-propan-2-ylbicyclo[3.1.0]hex-2-ene Chemical compound CC(C)[C@@]12C[C@@H]1[C@@H](C)C=C2 GJYKUZUTZNTBEC-IVZWLZJFSA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N 2,3,4,5-tetrahydroxypentanal Chemical compound OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
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- 230000004913 activation Effects 0.000 description 1
- IAJILQKETJEXLJ-RSJOWCBRSA-N aldehydo-D-galacturonic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-RSJOWCBRSA-N 0.000 description 1
- VYBREYKSZAROCT-UHFFFAOYSA-N alpha-myrcene Natural products CC(=C)CCCC(=C)C=C VYBREYKSZAROCT-UHFFFAOYSA-N 0.000 description 1
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- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
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- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 1
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- 239000008159 sesame oil Substances 0.000 description 1
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- 230000003068 static effect Effects 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a technique for extracting essential oil and pectin from plants, particularly a preparation technique for extracting essential oil and pectin from tangerine peel. The technique improves and optimizes the conventional extraction method in the prior art, boldly adopts the steps of ethanol treatment, ultraviolet irradiation, salt ion aging and the like, and effectively combines and optimizes the reaction parameters, thereby enhancing the output efficiency of essential oil and pectin and having wide application prospects.
Description
Technical field
The present invention relates to a kind of Technology of extracting pectin and volatile oil from plant, be specifically related to a kind of fabricating technology that extracts pectin and volatile oil from orange peel.
Background technology
China is the main place of production of orange, and cultivated area ranks first in the world, and output occupies third place in the world, orange aboundresources, and improved seeds are various, have the cultivation history of more than 4000 year.As far back as Xia dynasty's (front 21 century～front the 17th century), the citrus that the ground such as the Jiangsu, Anhui, Jiangxi, Hunan, Hubei of China produce, has classified the thing of tribute and taxes as.Through long-term cultivation, selection, citrus has become the mankind's precious fruit.Orange peel is the byproduct after orange processing, more account for whole fruit heavy 25%～40%, in orange peel, pectin content can reach 10%-30%.By the orange resource of China's abundant, from orange peel, extract pectin, just can turn waste into wealth, promote the development of local economy, break away from the situation that agricultural benefit is low, the output value is low, greatly improve the economic benefit of orange industry.
Volatile oil is present in orange or the tiny gland of peel of Citrus reticulata Blanco, is the significant by-products in orange or oranges and tangerines processing.Be widely used in the production of seasonings, beverage, food, makeup, tobacco and wine goods, soap, pharmaceutical products and sterilant.Have in recent years bibliographical information, volatile oil has to be made the effect of human central nervous calmness and alleviates irritable effect, can make people's Ginseng Extract, and wherein contained micro-tonka bean camphor has obvious antitumous effect.Its anticancer mechanism is the poisonous functional group of decompose carcinogenic substances the metabolism activation that suppresses cancerous tumor cell.
Prior art discloses the method for multiple extraction volatile oil or pectin, and for example steam distillation and milling process extract orange peel essential oil, and its extraction yield is generally in 1.5-3.5% left and right.But steam distillation is because service temperature is higher, can cause the thermolysis of thermographic compound in essential oil and the hydrolysis of facile hydrolysis composition and because thermal treatment meeting causes the loss of essential oil fragrance, milling process products obtained therefrom is impure, may there be moisture, chlorophyll, mucus etc., be difficult to essential oil completely to squeeze out simultaneously.Therefore this enriches cheap resource how to make full use of orange peel, has positive meaning.
CN1075729 discloses a kind of method from Orange Peel natural yellow pigment, mandarin oil and pectin.The method long flow path needs to use industrial chemicals sherwood oil in leaching process, because sherwood oil consumption is large, volatile, causes in production process solvent loss very large, and economic benefit is not high.And pericarp is a large amount of to be absorbed and residual organic solvent, and follow-up pectin extraction is brought inconvenience.CN2005100322627 discloses a kind of method of extracting mandarin oil and pectin from citrus peel, in the method leaching process, used industrial chemicals sherwood oil, caused in production process solvent loss very large, economic benefit is not high, remaining objectionable impurities, and sesame oil essence productive rate is low.Magazine " Shaoguan College's journal ", the improvement of extracting Obtaining Perfume Essential Oil from peel of Citrus reticulata Blanco, in September, 2004, discloses a kind of method of extracting volatile oil from orange peel, and multiple steps are improved; But its insufficient fragrance, complex process is not suitable for large-scale industrial production, and oil yield is lower.
The anxious one to be needed of prior art can effectively be extracted pectin and volatile oil, and the high processing technology that is applicable to technique simple possible of product output efficiency.
Summary of the invention
For the deficiencies in the prior art, the present invention improves and optimizes conventional extracting method of the prior art, has greatly improved the output capacity of pectin and the oil yield efficiency of volatile oil.
Technical scheme of the present invention completes as follows, specific as follows:
A method of extracting volatile oil and pectin from orange peel, comprises following operation steps:
4) orange peel of selecting fresh nothing to go mouldy, the dry place that puts into cool place, ventilation is for subsequent use;
5) get step 1) orange peel 100g be immersed in 1L calcium carbonate saturated aqueous solution 24 hours, pull post-flush out clean;
6) orange peel is cut into the square fragment of about 5mm, puts into volume fraction and be 70% ethanol and soak 30-40 minute, decompression rotary evaporation is removed ethanol;
4) ultraviolet ray is lower irradiates 15-30 minute, sends in expeller, adds pH adjusting agent 100ml when squeezing, and the component of pH value conditioning agent is: 0.2mol/L NaCl and 0.1mol/L NaHCO3;
5) will after extract filtration, get filtrate, filter residue takes out the production technique for follow-up other products; According to filtrate: the volume ratio that metabisulfite solution is 10: 1 is added the metabisulfite solution that quality volume fraction is 5%, at the temperature of 4 DEG C, leave standstill three days, after oily water separation thoroughly, extract the volatile oil on upper strata; Collect water and the filter residue of lower floor;
6) join in stainless steel heating tank after lower floor's water and filter residue are fully mixed, add the water of 10 times of volumes to stir and obtain solution A;
7) slowly add the ammonium oxalate of 1% (weightmeasurement ratio), wherein solution A: the volume ratio of ammonium oxalate is 1: 10, is slowly heated to 80 DEG C while stirring, keep 80 DEG C at 1 hour, then filter, collect filter residue for subsequent use;
8) under temperature is 60 DEG C, pH2, pressure 0.2Mpa condition, utilize vacuum concentrating apparatus concentrated, while being concentrated to 15% left and right of stoste volume, concentrated solution being emitted and be cooled to rapidly 4 DEG C;
9) according to 90% ethanol: the volume ratio that concentrated solution is 1: 1 adds 90% ethanol, stir while adding evenly, then leave standstill 6 hours; Vacuum filtration, reclaims filtrate, and 90% washing with alcohol for filter cake reclaims ethanol, filter cake is pulverized and be dried 2 hours at 50 DEG C, obtains pectin.
Embodiment
Below employing specific embodiment is made to further explanation to the present invention, but it is not as the restriction to initiative spirit of the present invention.
Embodiment 1
A method of extracting volatile oil and pectin from orange peel, comprises following operation steps:
1 orange peel of selecting fresh nothing to go mouldy, the dry place that puts into cool place, ventilation is for subsequent use;
2 get step 1) orange peel 100g be immersed in 1L calcium carbonate saturated aqueous solution 24 hours, pull post-flush out clean;
Orange peel is cut into the square fragment of 5mm by 3, puts into volume fraction and be 70% ethanol and soak 30 minutes, and decompression rotary evaporation is removed ethanol;
4 ultraviolet rays are lower irradiates 15 minutes, sends in expeller, adds pH adjusting agent 100ml when squeezing, and the component of pH value conditioning agent is: 0.2mol/L NaCl and 0.1mol/L NaHCO
3;
) will after extract filtration, get filtrate, filter residue takes out the production technique for follow-up other products; According to filtrate: the volume ratio that metabisulfite solution is 10: 1 is added the metabisulfite solution that quality volume fraction is 5%, at the temperature of 4 DEG C, leave standstill three days, after oily water separation thoroughly, extract the volatile oil on upper strata; Collect water and the filter residue of lower floor;
6) join in stainless steel heating tank after lower floor's water and filter residue are fully mixed, add the water of 10 times of volumes to stir and obtain solution A;
7) slowly add 1% ammonium oxalate, wherein solution A: the volume ratio of ammonium oxalate is 1: 10, is slowly heated to 80 DEG C while stirring, keep 80 DEG C at 1 hour, then filter, collect filter residue for subsequent use;
8) under temperature is 60 DEG C, pH2, pressure 0.2Mpa condition, utilize vacuum concentrating apparatus concentrated, while being concentrated to 15% left and right of stoste volume, concentrated solution being emitted and be cooled to rapidly 4 DEG C;
9) according to 90% ethanol: the volume ratio that concentrated solution is 1: 1 adds 90% ethanol, stir while adding evenly, then leave standstill 6 hours; Vacuum filtration, reclaims filtrate, and 90% washing with alcohol for filter cake reclaims ethanol, filter cake is pulverized and be dried 2 hours at 50 DEG C, obtains pectin.
Embodiment 2
A method of extracting volatile oil and pectin from orange peel, comprises following operation steps:
1 orange peel of selecting fresh nothing to go mouldy, the dry place that puts into cool place, ventilation is for subsequent use;
2 get step 1) orange peel 100g be immersed in 1L calcium carbonate saturated aqueous solution 24 hours, pull post-flush out clean;
Orange peel is cut into the square fragment of 5mm by 3, puts into volume fraction and be 70% ethanol and soak 40 minutes, and decompression rotary evaporation is removed ethanol;
4 ultraviolet rays are lower irradiates 30 minutes, sends in expeller, adds pH adjusting agent 100ml when squeezing, and the component of pH value conditioning agent is: 0.2mol/L NaCl and 0.1mol/L NaHCO
3;
) will after extract filtration, get filtrate, filter residue takes out the production technique for follow-up other products; According to filtrate: the volume ratio that metabisulfite solution is 10: 1 is added the metabisulfite solution that quality volume fraction is 5%, at the temperature of 4 DEG C, leave standstill three days, after oily water separation thoroughly, extract the volatile oil on upper strata; Collect water and the filter residue of lower floor;
6) join in stainless steel heating tank after lower floor's water and filter residue are fully mixed, add the water of 10 times of volumes to stir and obtain solution A;
7) slowly add 1% ammonium oxalate, wherein solution A: the volume ratio of ammonium oxalate is 1: 10, is slowly heated to 80 DEG C while stirring, keep 80 DEG C at 1 hour, then filter, collect filter residue for subsequent use;
8) under temperature is 60 DEG C, pH2, pressure 0.2Mpa condition, utilize vacuum concentrating apparatus concentrated, while being concentrated to 15% left and right of stoste volume, concentrated solution being emitted and be cooled to rapidly 4 DEG C;
9) according to 90% ethanol: the volume ratio that concentrated solution is 1: 1 adds 90% ethanol, stir while adding evenly, then leave standstill 6 hours; Vacuum filtration, reclaims filtrate, and 90% washing with alcohol for filter cake reclaims ethanol, filter cake is pulverized and be dried 2 hours at 50 DEG C, obtains pectin.
Embodiment 3
1, the volatile oil extracting by embodiment 1 and pectin fraction analysis:
Application GC-MS technical Analysis volatile oil component: D-limonene 81.17%, terpinene 6.27%, myrcene 2.96%, phantol 2.468%, 2-thujene 1.28%, terpinolene 1.046%, and other minor components.Find by detecting pectin extraction thing composition, galacturonic acid concentration 11.57, impurity: 3.41, pectin content 83.57, all the other are moisture.Adopt colorimetry of carbazole to measure its pectin content, measuring pectin content in orange peel is 22.65%.
2, appropriate Ethanol Treatment:
Adopt appropriate Ethanol Treatment, discharged greatly the solubility rate of volatile oil, and Ethanol Treatment step is before squeezing step, avoids sneaking in volatile oil; The impact of Ethanol Treatment step on volatile oil solubility rate: according to the operating method of embodiment 1, repeat ten batches, remove ten batches of the same repetitions of Ethanol Treatment step; We find, do not adopt the embodiment of Ethanol Treatment step, and productive rate is 7.18 ± 0.23g/kg orange peel; Adopt in the ethanol that volume fraction is 70% and soak after 30 minutes, productive rate improves greatly, up to 9.87 ± 0.51g/kg.
3, the UV treatment of suitable time:
Activated the enzyme in orange peel by suitable ultraviolet irradiation time, and in orange peel, cell walls is thoroughly destroyed, the various components such as volatile oil and pectin discharge to greatest extent; The present invention adopts ultraviolet ray and conventional milling process to combine, and has greatly improved the solubility rate of volatile oil and pectin.Find by simultaneous test, ultraviolet ray can improve the solubility rate of volatile oil and pectin greatly.Specifically with reference to table 1.
Table 1
4, rational salt ion ageing process:
We have adopted metabisulfite solution in static ageing process, possess salting out, and color and luster is good, and just, oil yield is high for fragrance.Wherein, blank group is not for adopting any salt ion ageing process, and other steps are identical.
The impact of table 2 metabisulfite solution on volatile oil:
5, adopt the improvement of the steps such as uv irradiating and vacuum concentration, the output of pectin is improved greatly, more than can reaching 22g/100g orange peel, in pectin extraction thing, pectin content is higher, moisture is lower, and it is evenly faint yellow that color is, and possesses good gellifying property and thickening power.
Be understandable that, the present invention can also make other restriction, and other of making on the basis of the embodiment of the present invention improve still within protection scope of the present invention.
Claims (1)
1. a method of extracting volatile oil and pectin from orange peel, is characterized in that, described method comprises following operation steps:
1) orange peel of selecting fresh nothing to go mouldy, the dry place that puts into cool place, ventilation is for subsequent use;
2) get step 1) orange peel 100g be immersed in 1L calcium carbonate saturated aqueous solution 24 hours, pull post-flush out clean;
3) orange peel is cut into the square fragment of 5mm, puts into volume fraction and be 70% ethanol and soak 30 minutes, decompression rotary evaporation is removed ethanol;
4) ultraviolet ray is lower irradiates 15 minutes, sends in expeller, adds pH adjusting agent 100ml when squeezing, and the component of pH value conditioning agent is: 0.2mol/LNaCl and 0.1mol/LNaHCO
3;
5) will after extract filtration, get filtrate, filter residue takes out the production technique for follow-up other products; According to filtrate: the volume ratio that metabisulfite solution is 10: 1 is added the metabisulfite solution that quality volume fraction is 5%, at the temperature of 4 DEG C, leave standstill three days, after oily water separation thoroughly, extract the volatile oil on upper strata; Collect water and the filter residue of lower floor;
6) join in stainless steel heating tank after lower floor's water and filter residue are fully mixed, add the water of 10 times of volumes to stir and obtain solution A;
7) slowly add 1% ammonium oxalate, wherein solution A: the volume ratio of ammonium oxalate is 1: 10, is slowly heated to 80 DEG C while stirring, keep 80 DEG C at 1 hour, then filter, collect filter residue for subsequent use;
8) under temperature is 60 DEG C, pH2, pressure 0.2Mpa condition, utilize vacuum concentrating apparatus concentrated, while being concentrated to 15% left and right of stoste volume, concentrated solution being emitted and be cooled to rapidly 4 DEG C;
9) according to 90% ethanol: the volume ratio that concentrated solution is 1: 1 adds 90% ethanol, stir while adding evenly, then leave standstill 6 hours; Vacuum filtration, reclaims filtrate, and 90% washing with alcohol for filter cake reclaims ethanol, filter cake is pulverized and be dried 2 hours at 50 DEG C, obtains pectin.
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| CN104031172A (en) * | 2014-06-03 | 2014-09-10 | 沈阳师范大学 | Method for extracting pectin from banana peel by ultrasonic synergistic ammonium oxalate method |
| CN105968227A (en) * | 2016-06-30 | 2016-09-28 | 潜山县有余瓜蒌开发有限责任公司 | Process of extracting pectin from snake gourd peel |
| RU2763401C1 (en) * | 2021-03-09 | 2021-12-28 | Евгений Михайлович Герасимов | Method for obtaining a pectin-containing composition |
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| CN102268327A (en) * | 2010-06-01 | 2011-12-07 | 浙江省柑桔研究所 | Method for orange peel essential oil and pectin combined production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268327A (en) * | 2010-06-01 | 2011-12-07 | 浙江省柑桔研究所 | Method for orange peel essential oil and pectin combined production |
Non-Patent Citations (2)
| Title |
|---|
| 李于善等.柑橘香精油的提取及提高其香气品质的研究.《食品与发酵工业》.2004,第30卷(第11期), |
| 柑橘香精油的提取及提高其香气品质的研究;李于善等;《食品与发酵工业》;20041130;第30卷(第11期);结论部分 * |
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| CN102796207A (en) | 2012-11-28 |
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