CN101830822A - Alcohol extraction process for extracting capsaicine in assistance of complex enzyme method - Google Patents
Alcohol extraction process for extracting capsaicine in assistance of complex enzyme method Download PDFInfo
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- CN101830822A CN101830822A CN200910068123A CN200910068123A CN101830822A CN 101830822 A CN101830822 A CN 101830822A CN 200910068123 A CN200910068123 A CN 200910068123A CN 200910068123 A CN200910068123 A CN 200910068123A CN 101830822 A CN101830822 A CN 101830822A
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Abstract
The invention provides an alcohol extraction process for extracting capsaicine in assistance of a complex enzyme method. The process comprises the steps of: firstly adding purified water in paprika, carrying out enzymolysis reaction on the paprika in the presence of a complex enzyme and suction-filtering; andcarrying out constant volume on the filtrate for later use by using edible alcohol, and extracting the capsaicine by reflux of 95% edible alcohol from paprika residues. The invention has the advantages that: 1. by carryng out compound processing on the paprika by using cellulose and pectinase by the ratio of 1:1 before alcohol extraction, the process achieves total capsaicine extraction rate 19.1% higher than that of a method which directly uses alcohol for extraction, can completely extract the capsaicine and reduce organic solvent consumption and extraction time; and 2. the process has low requirement on equipment, reduces production cost and is suitable to industrialized production.
Description
Technical field:
The present invention relates to a kind of extracting method of natural product, the processing method of the auxiliary alcohol extracting capsaicine of particularly a kind of combined-enzyme method.
Background technology:
The capsaicine traditional method is generally ethanol reflux extraction, acetone extraction method etc.Because capsicum has the rough structure of fibrous tissue of sheet, capsaicine and other fat-soluble components are present in the fibrous tissue, adopt traditional organic solvent extraction method need expend a large amount of organic solvents and time, and extraction efficiency is lower.Ultrasonic method, supercritical fluid extraction etc. are thought the novel method of natural product extraction, in the research that capsaicine extracts, think effectively, with traditional way relatively have the productive rate height, with short production cycle, need not heating, effective constituent advantage such as be not destroyed, but owing to reasons such as these method equipment requirements height, production cost height only are applied in the experimental study at present, difficulty is applicable to big industrial production.
Summary of the invention:
Purpose of the present invention just is to overcome above-mentioned the deficiencies in the prior art, and provide a kind of combined-enzyme method to assist the processing method of alcohol extracting capsaicine, after this method is utilized cellulase and polygalacturonase Combined Processing red chilly powder, extract capsaicine with Ethanol Method again, the extraction efficiency of capsaicine obviously is better than not adding the ethanol extraction method that enzyme is handled, and can all capsaicine have been carried.
Technical scheme of the present invention is: the processing method of the auxiliary alcohol extracting capsaicine of a kind of combined-enzyme method is characterized in that: at first add pure water in red chilly powder, then red chilly powder is carried out the enzyme digestion reaction of prozyme, suction filtration; Filtrate is with standby behind the edible ethanol constant volume, and the capsicum residue is with 95% edible ethanol refluxing extraction capsaicine.
The pure water that adds 10 times of quality volumes in the above-mentioned red chilly powder.
Above-mentioned prozyme is by the ratio combination in 1: 1 of polygalacturonase and cellulase.
The enzymolysis process condition of above-mentioned red chilly powder is: the chillies mass volume ratio is 10% o'clock, and the prozyme enzyme dosage is the 6-8mg/g capsicum, and hydrolysis temperature is 30-40 ℃, and the initial pH of enzymolysis solution is 4-6, and enzymolysis time is 1.8-2.2h.
The best enzymolysis process condition of above-mentioned red chilly powder is: the chillies mass volume ratio is 10% o'clock, and the prozyme enzyme dosage is the 8mg/g capsicum, and hydrolysis temperature is 40 ℃, and the initial pH of enzymolysis solution is 5.5, and enzymolysis time is 2h.
Above-mentioned extraction using alcohol condition is: 95% alcohol concn, to extract temperature be that 50 ℃, solid-liquid ratio are that 1: 11, extraction time are 1.5h, extracting liquid filtering, and extracting solution is standby with the ethanol constant volume, and spectrophotometry detects capsaicin content.
Advantage of the present invention is: 1, the present invention with cellulase and polygalacturonase by after 1: 1 Combined Processing red chilly powder, total extraction yield with Ethanol Method extraction capsaicine is higher by 19.1% than the extraction yield of the direct extraction of ethanol again, can all capsaicine have been carried, and reduce the consumption and the extraction time of organic solvent.2, not high to equipment requirements, reduced production cost, be fit to big industrial production.
Description of drawings:
Fig. 1 is the synoptic diagram of enzymolysis solution pH value to the influence of capsaicine output.
Fig. 2 is the synoptic diagram of hydrolysis temperature to the influence of capsaicine output.
Fig. 3 is the synoptic diagram of enzyme dosage to the influence of capsaicine output.
Fig. 4 is the synoptic diagram of enzymolysis time to the influence of capsaicine output.
Fig. 5 is the level of factor orthogonal test table
Fig. 6 is the present invention and the controlled trial table of enzymolysis ethanol extraction method capsaicine extraction yield not.
Embodiment:
1 materials and methods.
1.1 material and instrument.
Cluster redpepper (Tianjin Lan Shi seasonings company limited).Capsaicine reference substance (Chinese biological Products Co., Ltd), food grade ethanol (commercially available), other chemical reagent is analytical reagent.Prozyme is pressed combination (Hunan Youteer Biochemical Co., Ltd.) in 1: 1 by polygalacturonase and cellulase.
LC-IOATVP high performance liquid chromatograph day island proper Tianjin company); UV one 7220 type ultraviolet spectrophotometers (Beijing Rayleigh company).
1.2 test method.
1.2.1 the mensuration-spectrophotometry of capsaicin content.
Standardized solution preparation: accurately take by weighing the pure product 0.1000g of capsicine in the 100mL volumetric flask, dissolve and be diluted to scale with the 0.1mol/L sodium hydroxide solution, must capsicine standardized solution stock solution.Accurately move the 10.00mL standardized solution in the 100mL volumetric flask with transfer pipet, be diluted to scale, get capsicine standardized solution (100 μ g/mL) with the 0.1mol/L sodium hydroxide solution.
The preparation of phospho-wolframic acid molybdenum test solution: get sodium wolframate 10g and phospho-molybdic acid 2.4g, add water 70mL and phosphoric acid 5mL, reflux and to boil 2 hours, put coldly, thin up shakes up to 100mL, promptly.This liquid should be put in the Brown Glass Brown glass bottles and jars only, in the dark preserves.
Typical curve is drawn: draw capsicine standardized solution 0.50,1.00,2.00,4.00,6.00,8.00mL respectively in the 50mL volumetric flask, add 0.1mol/L sodium hydroxide solution 9.50,9.00,8.00,6.00,4.00 and 2.00mL more successively, then, in each volumetric flask, add 5mL phospho-wolframic acid-phosphorus molybdenum acid solution successively, after the jolting evenly, add about 30mL saturated sodium carbonate solution again, fully vibrate to the generation of adularescent precipitation, be settled to the 50mL scale with saturated sodium carbonate solution, leave standstill 2h after shaking up.Liquid centrifugation throw out will develop the color.With the reagent blank zeroing, the place measures with the 1cm cuvette at the 660nm wavelength, is X-coordinate with capsaicin concentration (X), and absorbancy (Y) is an ordinate zou, and it is as follows to get typical curve:
Y＝0.0226X+0.0084，R
2＝0.999。
Sample preparation: (capsicine content is settled to the 100mL scale 10～40mg) with the 0.1mol/L sodium hydroxide solution in the control 100mL volumetric flask, shakes up in the 100mL volumetric flask accurately to take by weighing 1～4g test portion (being accurate to 1mg).
Sample determination: draw above-mentioned sample solution 2.00mL in the 50mL volumetric flask, add 0.1mol/L sodium hydroxide solution 8mL, do blank simultaneously with 0.1mol/L sodium hydroxide solution 10mL.Press standard curve making method adding phospho-wolframic acid-phosphorus molybdenum acid solution and saturated sodium carbonate solution to the 50mL scale, leave standstill 2h after shaking up.Liquid centrifugation throw out will develop the color.Use the 1cm cuvette,, measure absorbancy, check in respective concentration, calculate the content of capsicine from typical curve at 660nm wavelength place with the reagent blank zeroing.
1.2.2 the enzyme solution of red chilly powder and the extracting method of capsaicine
Get the 1g dry paprika, add the pure water of 10 times of quality volumes, carry out the enzyme digestion reaction of prozyme under certain condition, suction filtration.Standby behind the filtrate usefulness edible ethanol constant volume.The capsicum residue is with 95% edible ethanol refluxing extraction capsaicine, the extraction using alcohol condition is: alcohol concn (95%), extraction temperature (50 ℃), solid-liquid ratio (1: 11), extraction time (1.5h), extracting liquid filtering, extracting solution is standby with the ethanol constant volume, and spectrophotometry detects capsaicin content.
The analysis of 2 red chilly powder enzyme solutions.
2.1 the influence (as shown in Figure 1) that enzymolysis pH value is extracted capsaicine.
Under the certain condition of enzymolysis time, hydrolysis temperature and enzyme dosage, the extraction efficiency of capsaicine is relevant with the pH variation of red chilly powder enzymolysis solution, its change curve such as Fig. 1.The content of capsaicine increases with the increase of enzymolysis damping fluid initial pH value earlier, reaches maximum value when pH=5.5; After the pH value was greater than 5.5, the content of capsaicine reduced with the increase of pH value on the contrary.The vigor that the plain enzyme of Mierocrystalline cellulose is described is subjected to the influence of environment pH value.In the pH value is 5.5 o'clock, and test is in best catalysis state with enzyme, helps the decomposition of Mierocrystalline cellulose and pectin and the release of capsaicine, and the proposition amount of capsaicine is the highest behind the enzymolysis.
2.2 the influence (as shown in Figure 2) that hydrolysis temperature extracts capsaicine.
In enzymolysis damping fluid initial pH value is 5.5, and under the certain condition of enzymolysis time and enzyme amount, the amount of extraction using alcohol capsaicine with the changing conditions of hydrolysis temperature as shown in Figure 2 behind the red chilly powder enzymolysis.The proposition amount of capsaicine begins to increase with the rising of hydrolysis temperature behind the test demonstration enzymolysis, reaches maximum in the time of 30～40 ℃; Rising with temperature after surpassing 40 ℃ reduces.Therefore, the enzymolysis test should be carried out at 30～40 ℃.
2.3 the influence (as shown in Figure 3) that enzyme dosage extracts capsaicine.
In enzymolysis damping fluid initial pH value is 5.5, and hydrolysis temperature is 40 ℃, and enzyme dosage to the influence of capsaicine extraction efficiency as shown in Figure 3.Test shows, under the certain condition of enzymolysis time, enzyme begins to increase along with the increase of enzyme dosage with the extracted amount of capsaicine; But after the ratio of enzyme dosage and red chilly powder reaches certain value, increase the consumption of enzyme again, the extraction output of capsaicine reduces on the contrary, this may be that excessive cellulase makes when reaction enzyme concn too high, be unfavorable for the molecular orientation motion, enzymic activity reduces on the contrary, and the capsaicine stripping is descended.Therefore, enzyme dosage is good with 8mg/g red chilly powder.
2.4 the influence (as shown in Figure 4) that enzymolysis time extracts capsaicine.
In enzymolysis damping fluid initial pH value is 5.5, and enzyme dosage is a 8mg/g red chilly powder, and hydrolysis temperature is 40 ℃, and the capsaicine extracted amount with the changing conditions of enzymolysis time as shown in Figure 4.Test shows that the extracted amount of capsaicine increases along with the increase of enzymolysis time; After enzymolysis time was greater than 2h, the extracted amount of capsaicine reduced on the contrary, and this may be the cause of capsaicine hydrolysis.Therefore, enzymolysis time is good about with 2h.
2.5 enzymolysis orthogonal test (as shown in Figure 5).
On the basis that above single factor is investigated, with 1g red chilly powder is that raw material carries out the test of four factors, three horizontal quadratures, with the capsaicine in its residue of 95% extraction using alcohol, serve as to investigate index with the proposition amount of capsaicine behind the enzymolysis, level of factor arrangement and test-results are as shown in Figure 5.
The extreme difference of orthogonal test (R) analysis revealed, enzymolysis solution initial pH value, hydrolysis temperature, enzyme dosage and enzymolysis time to the influence degree that capsaicine extracts are: enzyme dosage＞hydrolysis temperature＞enzymolysis solution initial pH value＞enzymolysis time.
In conjunction with single factor experiment and orthogonal experiments, the best enzymolysis process condition of the red chilly powder of originally determining is: the chillies mass volume ratio is 10% o'clock, prozyme enzyme dosage 8mg/g capsicum, 40 ℃ of hydrolysis temperatures, the initial pH 5.5 of enzymolysis solution, enzymolysis time 2h.
2.6 the prozyme pre-treatment is to the impact effect of different capsaicine extracting method
Enzymolysis red chilly powder is used alcohol concn (95%) again, is extracted temperature (50 ℃), solid-liquid ratio (1: 11), extraction time (1.5h) under the optimum enzymolysis condition of determining; Control group test is: do not add under the condition of prozyme and handle red chilly powder, residue with alcohol concn (95%), extract temperature (50 ℃), solid-liquid ratio (1: 11), extraction time (1.5h).Detect capsaicine proposition amount with spectrophotometry, test-results is shown in Figure 6.
As shown in Figure 6, the extraction efficiency of capsaicine obviously is better than not adding the ethanol extraction method that enzyme is handled after the combined-enzyme method processing red chilly powder, and extraction yield is high by 19.1%, can all capsaicine have been carried.
Claims (6)
1. the processing method of the auxiliary alcohol extracting capsaicine of combined-enzyme method is characterized in that: at first add pure water in red chilly powder, then red chilly powder is carried out the enzyme digestion reaction of prozyme, suction filtration; Filtrate is with standby behind the edible ethanol constant volume, and the capsicum residue is with 95% edible ethanol refluxing extraction capsaicine.
2. the processing method of the auxiliary alcohol extracting capsaicine of combined-enzyme method according to claim 1 is characterized in that: the pure water that adds 10 times of quality volumes in the above-mentioned red chilly powder.
3. the processing method of the auxiliary alcohol extracting capsaicine of combined-enzyme method according to claim 1 is characterized in that: above-mentioned prozyme is made up by polygalacturonase and the cellulase ratio by 1: 1.
4. the processing method of the auxiliary alcohol extracting capsaicine of combined-enzyme method according to claim 1, it is characterized in that: the enzymolysis process condition of above-mentioned red chilly powder is: the chillies mass volume ratio is 10% o'clock, the prozyme enzyme dosage is the 6-8mg/g capsicum, hydrolysis temperature is 30-40 ℃, the initial pH of enzymolysis solution is 4-6, and enzymolysis time is 1.8-2.2h.
5. the processing method of the auxiliary alcohol extracting capsaicine of combined-enzyme method according to claim 1, it is characterized in that: above-mentioned extraction using alcohol condition is: 95% alcohol concn, to extract temperature be that 50 ℃, solid-liquid ratio are that 1: 11, extraction time are 1.5h, extracting liquid filtering, extracting solution is standby with the ethanol constant volume, and spectrophotometry detects capsaicin content.
6. the processing method of the auxiliary alcohol extracting capsaicine of combined-enzyme method according to claim 4, it is characterized in that: the best enzymolysis process condition of above-mentioned red chilly powder is: the chillies mass volume ratio is 10% o'clock, the prozyme enzyme dosage is the 8mg/g capsicum, hydrolysis temperature is 40 ℃, the initial pH of enzymolysis solution is 5.5, and enzymolysis time is 2h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018242A (en) * | 2013-01-05 | 2013-04-03 | 西南大学 | Rapid colorimetric determination method for capsaicin content of capsicum products |
| CN103073915A (en) * | 2013-02-07 | 2013-05-01 | 湖南威嘉生物科技有限公司 | Process for extracting and separating capsanthin and capsaicin by using biological enzyme |
| CN109645426A (en) * | 2018-12-20 | 2019-04-19 | 四川大学 | A kind of coenzyme, which helps, extracts numb-taste components method |
| CN115530348A (en) * | 2022-10-09 | 2022-12-30 | 重庆德庄农产品开发有限公司 | Seasoning processing method based on enzymolysis |
| CN115553342A (en) * | 2022-09-09 | 2023-01-03 | 代代田(佛山)生物科技有限公司 | Chili oil and preparation method thereof |
| CN115644405A (en) * | 2022-11-08 | 2023-01-31 | 鸡泽县中调味业有限公司 | Nut chili oil and preparation method thereof |
| CN116098277A (en) * | 2022-12-28 | 2023-05-12 | 四川东坡中国泡菜产业技术研究院 | Method for improving utilization rate of peppers |
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2009
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Non-Patent Citations (2)
| Title |
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| 董新荣等: "纤维素酶预处理法提取辣椒素的研究", 《食品科学》 * |
| 袁唯等: "云南丘北辣椒中辣椒素酶法提取条件的优化", 《食品与发酵工业》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018242A (en) * | 2013-01-05 | 2013-04-03 | 西南大学 | Rapid colorimetric determination method for capsaicin content of capsicum products |
| CN103073915A (en) * | 2013-02-07 | 2013-05-01 | 湖南威嘉生物科技有限公司 | Process for extracting and separating capsanthin and capsaicin by using biological enzyme |
| CN103073915B (en) * | 2013-02-07 | 2014-08-20 | 湖南威嘉生物科技有限公司 | Process for extracting and separating capsanthin and capsaicin by using biological enzyme |
| CN109645426A (en) * | 2018-12-20 | 2019-04-19 | 四川大学 | A kind of coenzyme, which helps, extracts numb-taste components method |
| CN115553342A (en) * | 2022-09-09 | 2023-01-03 | 代代田(佛山)生物科技有限公司 | Chili oil and preparation method thereof |
| CN115530348A (en) * | 2022-10-09 | 2022-12-30 | 重庆德庄农产品开发有限公司 | Seasoning processing method based on enzymolysis |
| CN115644405A (en) * | 2022-11-08 | 2023-01-31 | 鸡泽县中调味业有限公司 | Nut chili oil and preparation method thereof |
| CN116098277A (en) * | 2022-12-28 | 2023-05-12 | 四川东坡中国泡菜产业技术研究院 | Method for improving utilization rate of peppers |
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Application publication date: 20100915 |