CN112961729B - Method for extracting peony hydrosol under optimized negative pressure distillation condition - Google Patents
Method for extracting peony hydrosol under optimized negative pressure distillation condition Download PDFInfo
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- CN112961729B CN112961729B CN202110315385.0A CN202110315385A CN112961729B CN 112961729 B CN112961729 B CN 112961729B CN 202110315385 A CN202110315385 A CN 202110315385A CN 112961729 B CN112961729 B CN 112961729B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
The invention relates to an extraction method, in particular to a method for extracting peony hydrosol under optimized negative pressure distillation conditions. Belongs to the technical field of skin care products. The extraction method of the optimal peony hydrosol after process optimization under the negative pressure condition comprises the following steps: the extraction pressure is 0.35MPa, the temperature is 90 ℃, the accumulated extraction time is 4 hours, and the feed-liquid ratio is 1: under the condition of 6, the extraction efficiency is highest, and the content of the main component is the largest.
Description
Technical Field
The invention relates to an extraction method, in particular to a method for extracting peony hydrosol under optimized negative pressure distillation conditions. Belongs to the technical field of skin care products.
Background
The solution with healing function obtained from different parts of the root, stem, leaf, flower, etc. of aromatic plant by water distillation is called pure dew. The existing method for extracting the peony hydrolat generally adopts normal pressure (under one atmosphere pressure) to carry out extraction by steam distillation, the steam distillation under the normal pressure usually needs high temperature of 100 ℃, the excessive temperature easily damages the secondary metabolite components of plants, the loss of active ingredients is caused, the fragrance of the hydrolat is also easily damaged, and the extraction efficiency of the common method under the normal pressure is lower, and the extraction rate and the content of the active ingredients are influenced.
Besides various rich colors such as powder, white, yellow, purple and the like, the peony flower has elegant and noble fragrance, the peony flower has rich and changeable fragrance, is strong and hot, has slight fragrance, has sweet fragrance and has herb fragrance, and the secondary metabolites directly related to the peony flower fragrance are terpene compounds and phenylpropane compounds.
Disclosure of Invention
The invention aims to provide a method for extracting peony hydrolat under optimized negative pressure distillation conditions, which has the characteristics of high extraction efficiency, maximum content of main components and the like.
The technical scheme of the invention is as follows: a method for extracting peony hydrosol under optimized negative pressure distillation conditions is provided, which adopts a negative pressure distillation method to extract peony petals to obtain peony hydrosol.
Further, the method for extracting peony hydrolat under optimized negative pressure distillation conditions comprises the following steps:
1) Picking peony petals and preprocessing;
1) Adding water into pretreated peony petals, and placing the pretreated peony petals into a round-bottom flask;
2) Adding distilled water in a certain proportion, and performing steam condensation reflux distillation on peony petals to extract peony hydrosol;
further, the ratio of peony petals to distilled water required for extraction is 1:6.
further, the steam vessel extraction pressure was 0.35MPa.
Further, the extraction temperature was 90℃and the total extraction time was 4 hours.
Further, the peony petals are the peony petals which are not scattered in the full bloom stage.
Further, the components for extracting the peony hydrosol comprise: alpha-myrcene, right-handed-limonene, alpha-ocimene, linalool, nonanal, trans-rose oxide, cis-trans-2, 6-nonanal, cis-2-nonanal, 1-nonanol, geraniol, neral, citral, citronellol, 1,3, 5-trimethoxybenzene, pentadecane, hexadecane, eicosane, 2-heptanol, 6-methyl-5-heptan-2-one, ethyl benzoate, isoneral, alpha-terpineol, 3-ethyl-3-pentanol, 1, 4-dimethoxybenzene, butylhydroxytoluene, aromatic alcohol acetate, caryophyllene.
The invention has the advantages that: according to the invention, conditions such as extraction pressure, extraction temperature, extraction time and feed-liquid ratio are optimized by negative pressure distillation, so that the extraction pressure is 0.35MPa, the temperature is 90 ℃, the cumulative extraction time is 4 hours, and the feed-liquid ratio is 1: under the condition of 6, the extraction efficiency is highest, and the content of the main component is the largest.
Detailed Description
1. Extraction of
The invention relates to a method for extracting peony hydrolat under optimized negative pressure distillation conditions.
The method specifically comprises the following steps:
1) Placing peony petals in a steam container;
2) Introducing water vapor, distilling the peony petals, and extracting peony hydrosol; wherein the extraction pressure of the steam container is 0.35MPa, the temperature is 90 ℃, the accumulated extraction time is 4 hours, and the mass ratio of the extracted peony hydrosol to the feed liquid is 1:6.
the peony petals are the peony petals which are not scattered in the full bloom stage.
The components for extracting the peony hydrosol comprise: alpha-myrcene, right-handed-limonene, alpha-ocimene, linalool, nonanal, trans-rose oxide, cis-trans-2, 6-nonanal, cis-2-nonanal, 1-nonanol, geraniol, neral, citral, citronellol, 1,3, 5-trimethoxybenzene, pentadecane, hexadecane, eicosane, 2-heptanol, 6-methyl-5-heptan-2-one, ethyl benzoate, isoneral, alpha-terpineol, 3-ethyl-3-pentanol, 1, 4-dimethoxybenzene, butylhydroxytoluene, aromatic alcohol acetate, caryophyllene.
2. The extraction process is preferably
And (3) optimizing extraction conditions: the single factor experiment design is that the main component (the relative content of the measured component is 1-10 -2 ) The content is a response value. Table 1 is the designed optimization parameters. See Table 1
| Level/factor | Extraction pressure/MPa | Cumulative extraction time/min | Extraction temperature/. Degree.C | Ratio of extracted liquid to solid |
| 1 | Atmospheric pressure 0.1 | 60 | 70 | 1：4 |
| 2 | Negative pressure 0.3 | 120 | 80 | 1：6 |
| 3 | Negative pressure 0.35 | 180 | 90 | 1：8 |
| 4 | / | 240 | 100 | 1：10 |
| 5 | / | 300 | / | / |
| 6 | / | 360 | / | / |
| 7 | / | 420 | / | / |
3. Headspace solid-phase microextraction method for determining main component types and content
Taking 1m L pure dew sample liquid, adding 10 mu L of 0.05 mu L/mL of 3-octanol as an internal standard, adopting a headspace solid-phase microextraction method to carry out gas chromatography-mass spectrometry combined detection, and carrying out component analysis to generate a total ion flow chromatogram (TIC). The Retention Index (RI) was calculated by calculating the retention time of the injected normal paraffins (C6-C30) at the same experimental conditions, comparing their RI with the retention index reported in the literature to identify compounds, and search matching the mass spectrum recorded by them with the data stored in the NIST02 spectrum database to identify the individual components of the peony hydrosol, the relative content of which was calculated using peak area normalization.
Chromatographic conditions:
TG-5MS chromatographic column (30 m. Times.0.25 mm. Times.0.25 um); the temperature of the sample inlet is 260 o C, performing operation; the carrier gas was helium (99.99% purity) and the column flow was 1.00m L/min. Column programming temperature: onset temperature 40 o C, hold for 3min, 3 o The C/min rate rises to 210 o C, maintaining for 2min, and then adding 20 o The C/min rate rises to 290 o C, maintaining for 8min, and running for 73.73min; the sample injection amount is 1 mu L, and the split ratio is 5ml/min.
Mass spectrometry conditions: electron bombardment ionization source, electron energy 70e V; ion source temperature 230 o C, interface temperature 280 o C, scanning quality ranges from 40 to 600amu.
Analysis of results:
table 2: analysis of main components of peony petal pure dew under different extraction pressures
As shown in Table 2, under different pressure conditions, the main component substances (relative content is 1-10 -2 ) There are 17 kinds in total, and the optimum extraction pressure in the negative pressure steam distillation was found to be 0.35MPa, since the content of 10 kinds of main components reached the highest value under the pressure condition of 0.35MPa.
Table 3: analysis of main components of peony petal pure dew under different extraction temperatures
As shown in Table 3, under different temperature conditions, the main component substances (relative content is 1-10 -2 ) There are 15 kinds in total, and the optimum extraction temperature in the negative pressure steam distillation was found to be 90℃because the maximum value of the 14 kinds of main components was reached at 90 ℃.
Table 4-1: analysis (absolute content) of main components of peony petal hydrosol under different accumulated extraction time
Table 4-2: analysis (relative content) of main components of peony petal hydrosol under different accumulated extraction time
As shown in tables 4-1 and 4-2, under the condition of different accumulated extraction time, the main component substances (relative content is 1-10 -2 ) There are 19 kinds in total. Among them, 14 main component substances were found to have a cliff-like decrease in the main component content from the 5 th hour, and the extraction efficiency was significantly decreased, so that the optimum cumulative extraction time in the negative pressure steam distillation was found to be 4 hours.
Table 5: analysis of main components of peony petal pure dew under different extraction liquid ratios
As shown in Table 5, as shown in Table 3, under the condition of different feed-to-liquid ratios, the main component substances (relative content is 1-10 -2 ) There are 12 kinds of the materials, wherein the ratio of the materials to the liquid is 1:6, the content of 11 main components reaches the highest value, so that the optimal extraction liquid-to-liquid ratio in the negative pressure steam distillation is known to be 1:6.
therefore, the invention provides a method for extracting peony hydrolat under the optimized negative pressure distillation condition, which is an optimal peony hydrolat extraction method after process optimization under the negative pressure condition, and comprises the following steps: the extraction pressure is 0.35MPa, the temperature is 90 ℃, the accumulated extraction time is 4 hours, and the feed-liquid ratio is 1: under the condition of 6, the extraction efficiency is highest, and the content of the main component is the largest.
Claims (1)
1. A method for extracting peony hydrosol under optimized negative pressure distillation conditions is characterized by comprising the following steps: the method adopts a negative pressure distillation method to extract peony petals to obtain peony hydrosol; the method specifically comprises the following steps:
1) Placing peony petals in a steam container;
2) Introducing water vapor, distilling the peony petals, and extracting peony hydrosol; wherein the extraction pressure of the steam container is 0.035MPa, the temperature is 90 ℃, the accumulated extraction time is 4 hours, and the mass ratio of the extracted peony hydrosol to the feed liquid is 1:6, preparing a base material;
the peony petals are peony petals which are not scattered in the full bloom stage;
the components for extracting the peony hydrosol comprise: alpha-myrcene, right-handed-limonene, alpha-ocimene, linalool, nonanal, trans-rose oxide, cis-trans-2, 6-nonanal, cis-2-nonanal, 1-nonanol, geraniol, neral, citral, citronellol, 1,3, 5-trimethoxybenzene, pentadecane, hexadecane, eicosane, 2-heptanol, 6-methyl-5-heptan-2-one, ethyl benzoate, isoneral, alpha-terpineol, 3-ethyl-3-pentanol, 1, 4-dimethoxybenzene, butylhydroxytoluene, aromatic alcohol acetate, caryophyllene.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060084083A (en) * | 2005-01-17 | 2006-07-24 | 경북대학교 산학협력단 | Methods for increasing paeonol content in moutan cortex, and the method for extraction of paeonol having increased contents obtained by the method |
| CN103194312A (en) * | 2013-03-24 | 2013-07-10 | 西北农林科技大学 | Method for extracting essential oil from cypress leaves |
| CN103305344A (en) * | 2013-06-18 | 2013-09-18 | 菏泽尧舜牡丹生物科技有限公司 | Method for extracting peony essence from fresh peony flowers |
| CN104087424A (en) * | 2014-08-04 | 2014-10-08 | 安阳市晶华油脂工程有限公司 | Method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers |
| CN105779136A (en) * | 2016-05-28 | 2016-07-20 | 黄宇松 | Peony flower essential oil extracting method |
| CN106929153A (en) * | 2016-04-29 | 2017-07-07 | 深圳市大百汇技术有限公司 | A kind of preparation method and applications of rosemary hydrosol |
| KR20180080737A (en) * | 2017-01-04 | 2018-07-13 | (주)마블러 | Wet tissue comprising extracts of medical palnt, moringa seed, bean and rice |
| CN110128238A (en) * | 2019-06-05 | 2019-08-16 | 武汉工程大学 | A method of entrainment extracts and overcritical isolates and purifies squalene from Grain Production of Amaranthus seed |
| CN110742836A (en) * | 2019-12-12 | 2020-02-04 | 广州丹荟生物科技有限公司 | Peony stock solution skin-refreshing mask and preparation method thereof |
| CN111481485A (en) * | 2020-06-15 | 2020-08-04 | 西北农林科技大学 | Peony bacteriostatic moisturizing hand cream and preparation method thereof |
| CN111830145A (en) * | 2020-03-10 | 2020-10-27 | 北京农业生物技术研究中心 | Method for determining feeding ratio and distillation time of black-branch rose hydrosol |
-
2021
- 2021-03-24 CN CN202110315385.0A patent/CN112961729B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060084083A (en) * | 2005-01-17 | 2006-07-24 | 경북대학교 산학협력단 | Methods for increasing paeonol content in moutan cortex, and the method for extraction of paeonol having increased contents obtained by the method |
| CN103194312A (en) * | 2013-03-24 | 2013-07-10 | 西北农林科技大学 | Method for extracting essential oil from cypress leaves |
| CN103305344A (en) * | 2013-06-18 | 2013-09-18 | 菏泽尧舜牡丹生物科技有限公司 | Method for extracting peony essence from fresh peony flowers |
| CN104087424A (en) * | 2014-08-04 | 2014-10-08 | 安阳市晶华油脂工程有限公司 | Method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers |
| CN106929153A (en) * | 2016-04-29 | 2017-07-07 | 深圳市大百汇技术有限公司 | A kind of preparation method and applications of rosemary hydrosol |
| CN105779136A (en) * | 2016-05-28 | 2016-07-20 | 黄宇松 | Peony flower essential oil extracting method |
| KR20180080737A (en) * | 2017-01-04 | 2018-07-13 | (주)마블러 | Wet tissue comprising extracts of medical palnt, moringa seed, bean and rice |
| CN110128238A (en) * | 2019-06-05 | 2019-08-16 | 武汉工程大学 | A method of entrainment extracts and overcritical isolates and purifies squalene from Grain Production of Amaranthus seed |
| CN110742836A (en) * | 2019-12-12 | 2020-02-04 | 广州丹荟生物科技有限公司 | Peony stock solution skin-refreshing mask and preparation method thereof |
| CN111830145A (en) * | 2020-03-10 | 2020-10-27 | 北京农业生物技术研究中心 | Method for determining feeding ratio and distillation time of black-branch rose hydrosol |
| CN111481485A (en) * | 2020-06-15 | 2020-08-04 | 西北农林科技大学 | Peony bacteriostatic moisturizing hand cream and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| "牡丹花精油的提取、分析及抗氧化性研究";李双;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20160215;全文 * |
| 杨朝飞等."附件二、某钢铁企业节能减排建设低碳绿色焦化厂的转型研究".《中国绿色经济发展机制和政策创新研究 下册》.中国环境科学出版社,2012,(第1版),第531页. * |
| 林玉萍等."实验五 减压蒸馏".《有机化学实验》.华中科技大学出版社,2020,(第1版),第82页. * |
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