CN102766535B - Method for extracting peony oil by water - Google Patents

Method for extracting peony oil by water Download PDF

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Publication number
CN102766535B
CN102766535B CN 201210270713 CN201210270713A CN102766535B CN 102766535 B CN102766535 B CN 102766535B CN 201210270713 CN201210270713 CN 201210270713 CN 201210270713 A CN201210270713 A CN 201210270713A CN 102766535 B CN102766535 B CN 102766535B
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extraction
water
peony
still
extracting
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CN102766535A (en
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梁小红
邵大晓
李俊峰
王锦娜
耿燕
宋慧娟
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People's livelihood Pharmaceutical Group Co., Ltd.
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HENAN SINO-AMERICAN BIOTECHNOLOGY Co Ltd
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Abstract

The invention belongs to the field of a peony oil extracting technology, and in particular relates to a method for extracting peony oil by water. The peony oil is obtained by placing the peony petals into an extraction kettle after being ground, adding 1-5 folds by weight of water, controlling the pressure of the extraction kettle to 5-30Mpa, temperature to 100-300 DEG C and extraction time to 5-120 min, separating to obtain an extracting solution, cooling the extracting solution to 100 DEG C, performing oil water separation, and collecting the oily matters. A high-temperature high-pressure extraction process provided by the invention is capable of very quickly obtaining the peony oil, and also has the advantages of being free of an organic solvent, clearer process, more friendly environment, faster extracting speed, higher efficiency, simpler technology, and lower equipment and operation cost.

Description

A kind of method with water extraction Tree Peony flower oil
Technical field
The invention belongs to tree peony caul-fat extractive technique field, particularly a kind of method with water extraction Tree Peony flower oil.
Background technology
Tree peony is the Ranunculaceae Paeonia, and machaka is distributed widely in Henan, Shandong, Anhui, Shaanxi, Sichuan, zhejiang and other places, especially with Luoyang, the plantation of two places, Heze at most.
The large-scale U.S. of Tree Peony flower, elegant and poised, the light uniqueness of the fragrance of a flower are traditional famous flowers of China, and the beginning contains in Tang, and " unsurpassed " Song Yu is thriving and prosperous, lucky rich and honour symbol, are described as king aromatic, in spending.
Contain micro-natural flavor material and terpenes, hydrocarbon compound in the Tree Peony flower, as geraniol, Geraniol, phantol etc., health-care effects such as calmness, anti-inflammatory, endocrine regulation are arranged.But because content is very little and molecular weight is little, volatile, be difficult for, so expensive.The peony essential oil of Xiao Shouing mostly is composite or the chemosynthesis gained in the market, and life-time service is unfavorable to skin.
Few to the extraction research of tree peony caul-fat at present, the finding extracting method has distillation method (extraction of peony essential oil from water vapour by distillation and the application CN200710189719.4 in perfuming cigarette thereof), petroleum ether extraction method (peony extraction extracted from petroleum ether and the application CN200710189718.X in perfuming cigarette thereof) and supercritical CO 2Extraction process (a kind of supercritical CO 2The method CN200810049972.4 of abstracting tree peony volatile oil; A kind of supercritical extraction method of peony essential oil and application CN201110302946.X thereof) etc.What extraction efficiency was the highest is supercritical CO 2Extraction process.But these extracting method complex steps, extraction efficiency is not high, is not suitable for big production requirement.
Summary of the invention
The object of the present invention is to provide a kind of method with water extraction Tree Peony flower oil, this method required time is short, the friendly environmental protection of solvent, and process is simple.
For achieving the above object, the technical scheme taked of the present invention is as follows:
A kind of method with water extraction Tree Peony flower oil: extract in the still packing into after the peony petal pulverizing, add water 1-5 times of weight, it is that 5-30Mpa, temperature are 100-300 ℃ that still pressure is extracted in control, extraction time is 5-120 minute, separate and obtain extracting solution, it is cooled to below 100 ℃, and oily water separation is collected oily matter and is namely got the tree peony caul-fat.
Preferably, it is 100-200 ℃ that the still temperature is extracted in control, and extraction time is 5-60 minute.
Further preferably, described peony petal is half-open to peony petal in full bloom.
Again further preferably, peony petal is crushed to particle diameter at 20 ~ 60 orders.
Still more preferably, will pulverize again after peony petal cleaning, the drying.
Water extraction of the present invention is operated and can be realized in the conventional High Temperature High Pressure extraction in this area equipment, need not to purchase in addition special equipment.
Water is the extraction solvent of an environmental sound.Under the normal temperature and pressure, the polarity of water is very big, can dissolve polar organic compound well, but then very little to Semi-polarity and nonpolar organic compound solubleness.Along with the rising of temperature, the polarity of water can reduce, to the dissolving power increase of Semi-polarity and nonpolar organic matter.
Under the pressure of appropriateness, when water was heated to 100-374 ℃ sub-critical temperature, the polarity of liquid water can vary with temperature and change, and more is similar to organic solvent, and the dissolving power of Semi-polarity and nonpolar organic matter is strengthened greatly.As being 250 ℃ when temperature, during pressure l0MPa, polarity and the methyl alcohol of liquid water are suitable.
The boiling point of Vegetable oil lipoprotein is generally 170-300 ℃, adopts High Temperature High Pressure water extraction method of the present invention can make the grease stripping complete, and extraction yield can be up to more than 1%.Compare with distillation and extraction method, yield is higher; Compare with the organic solvent extraction method, not with an organic solvent, avoided the organic solvent residual of pollution and extract; Compare with supercritical carbon dioxide extraction, do not use the carbonic acid gas that can produce Greenhouse effect, and the efficient height, extraction time is also short.
High Temperature High Pressure water extraction of the present invention can very rapidly obtain the tree peony caul-fat, has without the need for machine solvent, process cleaning, environmental friendliness, advantage such as extraction rate is fast, efficient is high, technology is simple, equipment and running cost are lower, is embodied in:
(1) process is simple: present method mainly is divided into extraction and separated for two steps, water is pumped in the extraction still of the peony petal that pulverizing is housed, and certain hour is extracted in the back of heating up, and after the high temperature extraction liquid cooling but being discharged, oily water separation gets final product again;
(2) environmental protection: present method adopts water as solvent, just makes the water that extracts in the still keep subcritical state, and process makes the green process that grease extracts becomes a cleaner production more close to the pressure kettle poach food that uses in the family.
(3) extraction time is short: because the characteristic of water under High Temperature High Pressure, the stripping property of grease in the Tree Peony flower is had good promoter action, extraction time usually at several minutes to dozens of minutes;
(4) the grease stripping is complete: the intensification gradually of water (natural heating process) can be played gradient elution and similarly act on, and extracts fully, and yield is at 0.8-1.3%.
5) industrial application value: technology is simple, can mass-producing extract grease, has industrial application value.
Embodiment
Embodiment 1
A kind of method with water extraction Tree Peony flower oil, step is as follows:
(1) get the raw materials ready: it is half-open to peony petal in full bloom to pluck the field, and cleaning, crushed after being dried are crossed 20 mesh sieves, with the 10000g peony petal powder extraction still of packing into.
(2) extract: add water 2 times of weight, unlatching offers high-pressure pump and the control of extracting still and extracts still working pressure l0MPa, opens simultaneously and extracts still overcoat heating unit to 185 ℃, and the water that extract in the still this moment is in subcritical state, close and extract still front and back valve, keep 15 minutes extraction times.
(3) cooling: close heating power supply, open and extract still front and back valve, pump into water displacement high temperature extraction liquid by high-pressure pump, high temperature extraction liquid is cooled to rapidly below 100 ℃, oily water separation, and the oily matter of collecting 121.5g is the tree peony caul-fat, and extraction yield is 1.22%.
(4) wastage raffinate: will extract still mesohigh liquid discharge to normal pressure, and draw off the peony petal residue.
Embodiment 2
A kind of method with water extraction Tree Peony flower oil, step is as follows:
(1) get the raw materials ready: it is half-open to peony petal in full bloom to pluck the field, and cleaning, crushed after being dried are crossed 20 mesh sieves, with the 10000g peony petal powder extraction still of packing into.
(2) extract: add water 2 times of weight, unlatching offers high-pressure pump and the control of extracting still and extracts still working pressure 5MPa, opens simultaneously and extracts still overcoat heating unit to 150 ℃, and the water that extract in the still this moment is in subcritical state, close and extract still front and back valve, keep 5 minutes extraction times.
(3) cooling: close heating power supply, open and extract still front and back valve, pump into water displacement high temperature extraction liquid by high-pressure pump, high temperature extraction liquid is cooled to rapidly below 100 ℃, oily water separation, and the oily matter of collecting 80.5g is the tree peony caul-fat, and extraction yield is 0.81%.
(4) wastage raffinate: will extract still mesohigh liquid discharge to normal pressure, and draw off the peony petal residue.
Embodiment 3
A kind of method with water extraction Tree Peony flower oil, step is as follows:
(1) get the raw materials ready: it is half-open to peony petal in full bloom to pluck the field, and cleaning, crushed after being dried are crossed 20 mesh sieves, with the 10000g peony petal powder extraction still of packing into.
(2) extract: add water 2 times of weight, unlatching offers high-pressure pump and the control of extracting still and extracts still working pressure 5MPa, opens simultaneously and extracts still overcoat heating unit to 200 ℃, and the water that extract in the still this moment is in subcritical state, close and extract still front and back valve, keep 15 minutes extraction times.
(3) cooling: close heating power supply, open and extract still front and back valve, pump into water displacement high temperature extraction liquid by high-pressure pump, high temperature extraction liquid is cooled to rapidly below 100 ℃, oily water separation, and the oily matter of collecting 89.5g is the tree peony caul-fat, and extraction yield is 0.90%.
(4) wastage raffinate: will extract still mesohigh liquid discharge to normal pressure, and draw off the peony petal residue.
Embodiment 4
A kind of method with water extraction Tree Peony flower oil, step is as follows:
(1) get the raw materials ready: it is half-open to peony petal in full bloom to pluck the field, and cleaning, crushed after being dried are crossed 20 mesh sieves, with the 10000g peony petal powder extraction still of packing into.
(2) extract: add water 2 times of weight, unlatching offers high-pressure pump and the control of extracting still and extracts still working pressure 30MPa, opens simultaneously and extracts still overcoat heating unit to 180 ℃, and the water that extract in the still this moment is in subcritical state, close and extract still front and back valve, keep 45 minutes extraction times.
(3) cooling: close heating power supply, open and extract still front and back valve, pump into water displacement high temperature extraction liquid by high-pressure pump, high temperature extraction liquid is cooled to rapidly below 100 ℃, and the oily matter that 110.5g is collected in oily water separation is the tree peony caul-fat, and extraction yield is 1.11%.
(4) wastage raffinate: will extract still mesohigh liquid discharge to normal pressure, and draw off the peony petal residue.

Claims (5)

1. method with water extraction Tree Peony flower oil, it is characterized in that: pack into after peony petal is pulverized and extract in the still, add water 1-5 times of weight, it is that 5-30Mpa, temperature are 100-300 ℃ that still pressure is extracted in control, extraction time is 5-120 minute, separates to obtain extracting solution, and it is cooled to below 100 ℃, oily water separation is collected oily matter and is namely got the tree peony caul-fat.
2. the method for claim 1 is characterized in that: it is 100-200 ℃ that the still temperature is extracted in control, and extraction time is 5-60 minute.
3. method as claimed in claim 2 is characterized in that: described peony petal is half-open to peony petal in full bloom.
4. method as claimed in claim 3 is characterized in that: peony petal is crushed to particle diameter at 20 ~ 60 orders.
5. method as claimed in claim 4 is characterized in that: will pulverize after peony petal cleaning, the drying again.
CN 201210270713 2012-08-01 2012-08-01 Method for extracting peony oil by water Active CN102766535B (en)

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Publication number Priority date Publication date Assignee Title
CN103484256A (en) * 2013-10-11 2014-01-01 青岛农业大学 Method for extracting peony stamen volatile oil by using steam distillation
CN104004589B (en) * 2013-10-31 2017-02-08 菏泽中禾健元生物科技有限公司 Producing method of peony essential oil
CN106377582A (en) * 2016-08-31 2017-02-08 上海新亚药业高邮有限公司 Comprehensive extraction method of peony volatile oil and general flavone
CN110157543A (en) * 2019-04-25 2019-08-23 南京康之源农业科技发展有限公司 A kind of preparation method of peony essential oil
CN114437870A (en) * 2021-12-22 2022-05-06 广东石丰农业科技有限公司 Extraction preparation process of essential oil of Abelmoschus manihot

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CN101647872A (en) * 2009-09-07 2010-02-17 兰州牡丹园艺开发公司 Peony essential oil soft capsule and preparation method thereof
CN101812370A (en) * 2010-03-29 2010-08-25 甘肃省轻工研究院 Method and device for extracting peony seed oil from peony seeds

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