CN102000183B - Method for extracting flavone and pectin in series from dried orange peel - Google Patents
Method for extracting flavone and pectin in series from dried orange peel Download PDFInfo
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- CN102000183B CN102000183B CN201010562597A CN201010562597A CN102000183B CN 102000183 B CN102000183 B CN 102000183B CN 201010562597 A CN201010562597 A CN 201010562597A CN 201010562597 A CN201010562597 A CN 201010562597A CN 102000183 B CN102000183 B CN 102000183B
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- pericarpium citri
- citri reticulatae
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Abstract
The invention discloses a method for extracting flavone and pectin in series from dried orange peel, which comprises the following steps of: (1) treating raw materials, namely cutting the dried orange peel for later use; (2) performing alcohol extraction, namely extracting total dried orange peel flavone by refluxing in industrial alcohol; (3) filtering the solution in the (2), and concentrating the filtrate to obtain extract, wherein the main component of the extract is hesperidin by efficient liquid phase detection; (4) flushing the filter residue filtered from the (2) for two to three times by using tap water, adding tap water in an amount which is 10 to 30 times the weight of the filter residue, boiling the mixture, adjusting the pH value to between 1.5 and 2.0 by using hydrochloric acid, preserving the heat, and filtering the solution; (5) extracting the pectin from the filter residue in the (4) at the temperature of between 80 and 90 DEG C according to the method of the (4), and filtering the solution; and (6) combining the filtrate in the (4) and (5), concentrating the combined filtrate, settling the concentrate for 8 hours, filtering the solution, flushing the filter residue for two to three times by using 60 to 70 percent ethanol, and drying the filter residue at the temperature of 45 DEG C to obtain the pectin. The dried orange peel resource is fully utilized, the solvent extracted by the method is easily reclaimed for reuse, the energy consumption can be reduced during extracting the pectin with preserved heat, and aiming at the advantages of extraction and utilization of multiple components in the dried orange peel, the method is suitable for industrialized production of the total dried orange peel flavone and the pectin.
Description
Technical field
The invention belongs to the application technology purposes of Pericarpium Citri Reticulatae comprehensive utilization, specially refer to a kind of from Pericarpium Citri Reticulatae, the series connection and extract the method for flavone and pectin
Background technology
Pericarpium Citri Reticulatae is the outer peel of the drying and ripening of rutaceae orange (Citrus reticulate Blanco) and variety thereof, mainly contains pectin, flavonoid and volatilization wet goods composition.Present domestic part scholar has carried out the extraction process aspect to the flavone in the Pericarpium Citri Reticulatae and pectin and has studied, but on producing, remain in power consumption big, problem such as the low and method of yield is loaded down with trivial details.
Summary of the invention
It is the extraction that Pericarpium Citri Reticulatae carries out flavone and pectin that the present invention is primarily aimed at same material, provides a kind of from Pericarpium Citri Reticulatae, the series connection to extract the method for flavone and pectin.
The present invention seeks to realize through following technical scheme:
A kind of from Pericarpium Citri Reticulatae, the series connection extracted the method for flavone and pectin, may further comprise the steps:
(1), raw material handles: will dry Pericarpium Citri Reticulatae shred, subsequent use;
(2), alcohol extraction: use industrial alcohol to reflux, extract the Pericarpium Citri Reticulatae total flavones;
(3), (2) are filtered, filtrating concentrate extractum, main component detects through high performance liquid chromatogram and is Hesperidin;
(4), the filtering residue after (2) filtered is with tap water flushing 2-3 time, adds 10-30 tap water doubly, boils, and regulates pH value 1.5-2.0 with hydrochloric acid, insulation is filtered;
(5), filtering residue in (4) is extracted pectin, filtration according to the method for (4) in 80-90 ℃ again;
(6), the filtrating that merges in (4), (5) concentrates, precipitate with ethanol 8h filters, filtering residue is with 60-70% alcohol flushing 2-3 time, in 45 ℃, dry pectin.
Described from Pericarpium Citri Reticulatae series connection extract the method for flavone and pectin, step (2) solid-liquid ratio is 1: 10-1: 15, i.e. Pericarpium Citri Reticulatae: ethanol g/V is 1: 10-1: 15.
Described from Pericarpium Citri Reticulatae, the series connection extracted the method for flavone and pectin, and alcohol concentration is 95% in the step (2).
Described from Pericarpium Citri Reticulatae, the series connection extracted the method for flavone and pectin, and reflux temperature is 70 ℃ in the step (2), and return time is 2-3h.
Described from Pericarpium Citri Reticulatae, the series connection extracted the method for flavone and pectin, in the step (4), in 30-100 ℃, is incubated 1-24h, extracts again.
The present invention extracts pectin in order to fully utilize the Pericarpium Citri Reticulatae resource with 95% ethanol extraction total flavones and insulation.This method is extracted solvent and is prone to recycling, and the advantages such as extraction and application that pectin can reduce energy consumption and be directed against multiple old branch in the Pericarpium Citri Reticulatae are extracted in insulation, is suitable for the suitability for industrialized production of Pericarpium Citri Reticulatae total flavones and pectin.
Advantage of the present invention has the following aspects:
1, the present invention fully utilizes Pericarpium Citri Reticulatae, simultaneously content in the Pericarpium Citri Reticulatae more Flavonoid substances and pectin is extracted;
2, the present invention selects with 95% industrial alcohol the extraction of Flavonoid substances in the Pericarpium Citri Reticulatae to be helped the recycling of solution.
3, the present invention selects to boil the method for back in 30-100 ℃ of insulation 1-24h extraction Pericarpium Citri Reticulatae pectin, on producing, can reduce energy consumption, saves production cost;
4, the present invention is through adopting first heating extraction Flavonoid substances, and its heating helps the extraction of back pectin, and promptly when with the tap water being solvent extraction pectin, extraction ratio is more than 20%.
5, the present invention is through adopting first reflux, extract, Pericarpium Citri Reticulatae flavone class material, and the scheme of pectin is extracted in the back, and its pectin color and luster is superior to the pectin that directly from Pericarpium Citri Reticulatae, extracts, has promptly removed some coloring matters simultaneously during the reflux, extract, total flavones, helps the extraction of back pectin.
Description of drawings
Fig. 1 detects collection of illustrative plates for the standard substance high performance liquid chromatogram, and peak sequence is a naringin, Hesperidin, neohesperidin;
Fig. 2 detects collection of illustrative plates for extracting the sample high performance liquid chromatogram.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is elaborated.
Embodiment 1
Take by weighing the Pericarpium Citri Reticulatae 50g of oven dry, be chopped into the 5cm*5cm fritter,, the industrial alcohol with 95% is in 70 ℃ of backflow 3h, solid-liquid ratio be 1: 10 (Pericarpium Citri Reticulatae: 95% ethanol, g/V).Filter, filtrating concentrate extractum, the 150mg total flavones, detect through high performance liquid chromatogram and to be mainly Hesperidin.
The tap water of filtering residue with 10 times of amounts washed 2-3 time, add 30 times tap water, boil, regulate pH value 1.5-2.0, in 60 ℃, be incubated 4h, filter with hydrochloric acid.Filtering residue is extracted 1h, filtration again in 80-90 ℃.Merging filtrate concentrates, and the equal-volume dehydrated alcohol sink 8h, filters, and filtering residue is dried in 45 ℃ with 60-70% alcohol flushing 2-3 time, must 10.5g pectin.
Embodiment 2
Take by weighing the Pericarpium Citri Reticulatae 150g of oven dry, chopping, solid-liquid ratio is that (Pericarpium Citri Reticulatae: 95% ethanol, g/V), the industrial alcohol with 95% was in 70 ℃ of backflow 2h in 1: 15.Filter, filtrating concentrate extractum, total flavones 512mg.
Filtering residue with tap water flushing 2-3 time, is added 30 times tap water, boil, regulate pH value 1.5-2.0, in 70 ℃, be incubated 3h, filter with hydrochloric acid.Filtering residue is extracted 2h, filtration again in 80-90 ℃.Merging filtrate concentrates, and the equal-volume dehydrated alcohol sink 8h, filters, and filtering residue is dried in 45 ℃ with 60-70% alcohol flushing 2-3 time, must pectin 31.5g.
Embodiment 3
Take by weighing the Pericarpium Citri Reticulatae 250g of oven dry, chopping, solid-liquid ratio is that (Pericarpium Citri Reticulatae: 95% ethanol, g/V), the industrial alcohol with 95% was in 70 ℃ of backflow 2h in 1: 10.Filter, filtrating concentrate extractum, total flavones 965.3mg.
Filtering residue with tap water flushing 2-3 time, is added 30 times tap water, boil, regulate pH value 1.5-2.0 with hydrochloric acid, insulation 24h filters in 50 ℃.Filtering residue is extracted 2h, filtration again in 85 ℃.Merging filtrate concentrates, and the equal-volume dehydrated alcohol sink 8h, filters, and filtering residue is dried in 45 ℃ with 70% alcohol flushing 2-3 time, must pectin 52.7g.
Should be understood that, concerning those of ordinary skills, can improve or conversion, and all these improvement and conversion all should belong to the protection domain of accompanying claims of the present invention according to above-mentioned explanation.
Claims (1)
1. the method for extraction flavone and pectin of from Pericarpium Citri Reticulatae, connecting is characterized in that, may further comprise the steps:
(1), raw material handles: will dry Pericarpium Citri Reticulatae shred, subsequent use;
(2), alcohol extraction: use industrial alcohol to reflux, extract the Pericarpium Citri Reticulatae total flavones, solid-liquid ratio is 1: 10-1: 15, i.e. Pericarpium Citri Reticulatae: ethanol g/V is 1: 10-1: 15, alcohol concentration is 95%, reflux temperature is 70 ℃, return time is 2-3h;
(3), (2) are filtered, filtrating concentrate extractum, main component detects through high performance liquid chromatogram and is Hesperidin;
(4), the filtering residue after (2) filtered is with tap water flushing 2-3 time, adds 10-30 tap water doubly, boils, and regulates pH value 1.5-2.0 with hydrochloric acid, in 30-100 ℃, is incubated 1-24h, filter;
(5), filtering residue in (4) is extracted pectin, filtration according to the method for (4) in 80-90 ℃ again;
(6), the filtrating that merges in (4), (5) concentrates, precipitate with ethanol 8h filters, filtering residue is with 60-70% alcohol flushing 2-3 time, in 45 ℃, dry pectin.
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| CN201010562597A CN102000183B (en) | 2010-11-29 | 2010-11-29 | Method for extracting flavone and pectin in series from dried orange peel |
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| CN201010562597A CN102000183B (en) | 2010-11-29 | 2010-11-29 | Method for extracting flavone and pectin in series from dried orange peel |
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| CN102000183A CN102000183A (en) | 2011-04-06 |
| CN102000183B true CN102000183B (en) | 2012-10-10 |
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| CN103965371A (en) * | 2014-04-04 | 2014-08-06 | 施健 | Preparation process of pectin |
| CN103951722B (en) * | 2014-04-30 | 2017-01-18 | 湖南鑫利生物科技有限公司 | Method for jointly extracting hesperidin and pectin from citrus peels |
| CN105815708B (en) * | 2016-04-11 | 2019-10-25 | 重庆工商大学 | Preparation method and applications rich in pectin, the citrus peel residue Ultramicro-powder of general flavone |
| CN106214799B (en) * | 2016-08-01 | 2018-06-08 | 河北医科大学 | A kind of extracting method of orange peel general flavone |
| CN109096353A (en) * | 2018-08-08 | 2018-12-28 | 曹庸 | A kind of method that continuous phase transistion extracts aurantiamarin and pectin in citrus young fruit |
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Non-Patent Citations (7)
| Title |
|---|
| 何晋浙 |
| 何晋浙;等.柚皮中黄酮和果胶联产工艺的研究.《食品科技》.2004,(第7期),96-98. * |
| 等.柚皮中黄酮和果胶联产工艺的研究.《食品科技》.2004,(第7期),96-98. |
| 等.脐橙皮中黄酮类化合物与果胶的分离和提取研究.《分析测试技术与仪器》.2006,第12卷(第4期),239-242. |
| 蔡定建 |
| 蔡定建;何晋浙 * |
| 蔡定建;等.脐橙皮中黄酮类化合物与果胶的分离和提取研究.《分析测试技术与仪器》.2006,第12卷(第4期),239-242. * |
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