CN103254093A - Method for rapidly extracting capsaicin from pepper - Google Patents

Method for rapidly extracting capsaicin from pepper Download PDF

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Publication number
CN103254093A
CN103254093A CN201310199930XA CN201310199930A CN103254093A CN 103254093 A CN103254093 A CN 103254093A CN 201310199930X A CN201310199930X A CN 201310199930XA CN 201310199930 A CN201310199930 A CN 201310199930A CN 103254093 A CN103254093 A CN 103254093A
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ultrasonic
capsaicine
extraction
pepper
solid
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杨博智
周书栋
戴雄泽
马艳青
李雪峰
张竹青
陈文超
欧阳娴
弭宝彬
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杨博智
周书栋
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Abstract

The invention relates to a method for rapidly extracting capsaicin from pepper. The method comprises the following steps of: sample pretreatment: taking fresh pepper, removing dust, drying the pepper to constant weight to prepare dry pepper, removing stem and seed of the dry pepper, crushing peel and placenta into powder by using a crusher, and collecting dry pepper powder; and after ultrasonic extraction of the pepper powder, carrying out reduced pressure condensation on a capsaicin extracting solution to obtain a solid which is the capsaicin crude extract. The method for extracting the capsaicin from the pepper disclosed by the invention is simple, convenient, rapid, low in energy consumption, saved in cost, energy-saving, and environment-friendly. Furthermore, as the method provided by the invention has the advantages of simplicity, convenience, rapidness, high extraction efficiency, stability and reliability, the method is especially suitable for rapid and quantitative analysis of the capsaicin content in a sample to facilitate the monitoring on an intermediate link and the quality of a final product.

Description

A kind of from capsicum the method for rapid extraction capsaicine
Technical field
The present invention relates to the novel method that a kind of capsaicine extracts, more specifically relate to a kind of novel method of utilizing ultrasonic wave rapid extraction capsaicine from capsicum.
Background technology
Capsaicine is a kind of amide derivatives matter of separating from pepper fruit with pungent irritating vanillyl amine.The capsaicine chemical stability is higher, loss is minimum in various organic solvent extraction processes, have analgesia, antisepsis and anti-inflammation, anticancer, suppress tumour, regulate effects such as blood fat, appetite stimulator, promoting digestion, tear-gas, and because it belongs to the material of pure natural, the low murder by poisoning, pollution-free, be widely used in fields such as medicine, food, war industry, have very high social benefit and economic benefit.
The capsaicine extracting method is mainly organic solvent extraction, supercritical CO at present 2Extraction method, microwave extraction method, enzyme extraction method and solid phase extraction etc.Though wherein organic solvent extraction is fit to scale operation, the not high and leaching process of extraction yield takes time and effort.Supercritical CO 2Though extraction method, microwave extraction method, enzyme extraction method and solid phase extraction extraction yield height, preceding 2 kinds of method required equipment costlinesses, the extraction cost height, back 2 kinds of method complex operations, present 4 kinds of methods all also rest on the laboratory study stage.
Ultrasonic extraction utilizes the ultrasonic cavitation effect to produce enormous pressure moment to cause the principle of plant cell wall fragmentation to extract capsaicine, compare with above-mentioned 4 kinds of extracting method, have series of advantages such as easy and simple to handle, that extraction efficiency is high, extraction time is short, extract impurity is few.
People such as Li Mei powder disclose a kind of method of using ultrasonic wave to extract capsaicine from capsicum in " research of ultrasound-enhanced extraction capsaicine " [" Chinese seasonings " the 05th phase in 2005] literary composition, be evaluation index with the capsaicine extracted amount, adopt uniform design to determine the optimum extraction process parameter of ethanol ultrasonic extraction capsaicine: solid-liquid ratio is 1:5 (weightmeasurement ratio, g/ml), ultrasonic time is 40min, and ultrasonic power is 160W.
People such as Ursidae disclose a kind of method of using ultrasonic wave to extract capsaicine from capsicum in " researchs of supersound extraction capsaicine processing condition " [" modern food science and technology " 2006 the 22nd the 4th phases of volume] literary composition, adopt the orthogonal experiment design to determine to use methyl alcohol: the optimal processing parameter that tetrahydrofuran (THF) (volume ratio is 1:1) extracts capsaicine is: solid-liquid ratio 1:5 (weightmeasurement ratio, g/ml), ultrasonic temperature: 60 ℃, ultrasonic time 45min, ultrasonic power 100w extracts 3 times.
People such as Sun Yanxia disclose a kind of method of using supersonic method to extract capsaicine from capsicum in " research of ultrasonic extraction cluster redpepper capsaicine processing condition " [" Chengdu University journal (natural science edition) " 2009 the 28th the 3rd phases of volume] literary composition, extracted amount with capsaicine is evaluation index, adopt the definite optimal processing parameter with the extraction using alcohol capsaicine of orthogonal experiment design to be: solid-liquid ratio 1:5 (weightmeasurement ratio, g/ml), ultrasonic time 40min, ultrasonic power 120W.
Although preceding prior art is done a lot of work in the capsaicine research in using the ultrasonic extraction method capsicum, but mainly concentrating on, its research emphasis improves the extraction process aspect, and do not study in great detail for capsaicine extract part in the preparation method of chillies and the chillies, and the ultrasonic extraction process parameter relates to shortcomings such as ultrasonic time is long partially, ultrasonic power is bigger than normal in the prior art, time consumption and energy consumption has increased extraction cost.
Therefore, extraction process when being necessary in fact by comprehensive research ultrasonic extraction method capsaicine, comprise: chillies preparation, extract part screening, capsicum powder diameter are determined, are extracted solvent screening, ultrasonic extraction process parameter (solid-liquid ratio, ultrasonic temperature, ultrasonic time, ultrasonic power, ultrasonic number of times) is optimized, thus develop a kind of rapidly, less energy-consumption ground extracts the method for capsaicine.
Summary of the invention
For solving prior art problems, the present invention studies the extraction process that ultrasonic method is extracted capsaicine comprehensively, comprise: chillies preparation, extract part screening, capsicum powder diameter are determined, are extracted solvent screening, ultrasonic extraction process parameter (solid-liquid ratio, ultrasonic temperature, ultrasonic time, ultrasonic power, ultrasonic number of times) is optimized, thus develop a kind of rapidly, less energy-consumption ground extracts the method for capsaicine.
For realizing purpose of the present invention, the technique means that the present invention adopts be to provide a kind of from capsicum the method for rapid extraction capsaicine, comprise the steps:
1) get fresh chilli, dust is dried to constant weight;
2) go handle to remove seed, get pericarp and the placenta of chillies;
3) crushing screening is collected dry paprika;
4) extract: get dry paprika and add the organic solvent supersound extraction, filter, get the capsaicine extracting solution;
5) aftertreatment: the capsaicine extracting solution is concentrated into solid state, namely gets the capsaicine crude extract.
Be surprised to find that the present invention is by choosing specific extract part, namely pericarp and placenta can realize more accurate, stable and extract fast.
In one embodiment, the method for preparing chillies described in the step 1) is after wet gauze is wiped clean the fresh chilli surface, to be dried to constant weight under 60 ℃.Temperature is too high unfavorable to the chillies quality, and it is long that temperature is crossed low preparation chillies required time, and therefore, preparation chillies optimal temperature is about 60 ℃.
In another specific embodiment, the dry paprika size is can 100% to cross 40 mesh sieves in the step 3), and described sieve is standard medicine sieve, i.e. the standards of pharmacopoeia sieve.
Preferably, organic solvent described in the step 4) is methyl alcohol.
Preferably, the parameter of ultrasonic extraction process described in the step 4) is: and solid-liquid ratio 1:80-1:120 (weightmeasurement ratio, g/ml), ultrasonic temperature 40-60 ℃, ultrasonic time 10-30min, ultrasonic power 60-100W, extraction time 1-2 time.In one embodiment, the parameter of ultrasonic extraction process described in the step 4) is: solid-liquid ratio 1:100(weightmeasurement ratio, g/ml), 54 ℃ of ultrasonic temperature, ultrasonic time 18min, ultrasonic power 60W, extraction time 2 times.
In a preferred embodiment, the condition of the plain extracting solution of concentrated pepper described in the step 5) is: pressure 0.08MPa, 50 ℃ of temperature are concentrated into solid.In some embodiments, described solid water content is below the 10wt%, below the preferred 5wt%.
The useful technique effect that the present invention obtains comprises at least: provide a kind of from capsicum the method for rapid extraction capsaicine, determined from capsicum, to extract the efficient part of capsaicine, be pericarp and placenta, optimized the method for preparing chillies, the optimal temperature of preparation chillies and the extraction process parameter of having optimized the ultrasonic extraction capsaicine have been determined, adopt this method to extract capsaicine, simple and efficient, energy consumption is low, save cost, be a kind of fast, energy-saving and environmental protection extract the method for capsaicine in the capsicum.In addition and since the present invention have easy fast, extraction yield is high, the advantage that method is reliable and stable, thus be particularly suitable for capsaicin content in the fast quantitative analysis sample, be convenient to the monitoring of middle-chain and end product quality.
Embodiment
For making the present invention easier to understand, describe the present invention in detail below in conjunction with embodiment, these embodiment only play the illustrative effect, are not limited to range of application of the present invention, NM concrete experimental technique carries out according to the normal experiment method usually in the following example.
Placenta of the present invention refers to be attached with in the fruit of capsicum the position of chilli seed.
Embodiment 1: the screening of solid-liquid ratio of the present invention, ultrasonic temperature, ultrasonic time, ultrasonic power
Get the dry paprika of 40 mesh sieves, added methyl alcohol, the supersound extraction capsaicine.Be to investigate index with the capsaicin content, according to Box – Benhnken test design principle, choose solid-liquid ratio (1:80,1:100,1:120(weightmeasurement ratio, g/ml)), ultrasonic temperature (40,50,60 ℃), ultrasonic time (10,20,30min), ultrasonic power (60,80,100W) carry out the response surface analysis test, optimize the capsaicine extraction process, the result is as shown in table 1.
Table 1 response surface analysis scheme and result
Figure BDA00003240525200041
Testing data in the his-and-hers watches 1 is carried out progressively regression fit, gets regression equation: Y=-61.635+0.982 * 10 3A+0.273B+0.580C+0.096D+5.238AB-14.761AC-1.667AD-21.425 * 10 -3BC+8.750 * 10 -5BD-8.750 * 10 -5CD-4.547 * 10 5A 2-2.954 * 10 -3B 2-8.554 * 10 -3C 2-6.198 * 10 -4D 2(wherein Y is capsaicin content, and A is solid-liquid ratio, and B is ultrasonic temperature, and C is ultrasonic time, and D is ultrasonic power).Regression equation is analyzed, and the optimal processing parameter that gets the supersound extraction capsaicine is: and solid-liquid ratio 1:103 (weightmeasurement ratio, g/ml), 53.45 ℃ of ultrasonic temperature, ultrasonic time 18.64min, ultrasonic power are 63.26W, and prediction capsaicin content theoretical value is 6.20mg/g.Consider the limitation of actually operating, with the extraction process parameter be modified to solid-liquid ratio be 1:100 (weightmeasurement ratio, g/ml), ultrasonic temperature is that 54 ℃, ultrasonic time are 18min, ultrasonic power is 60W.The actual capsaicin content value that records is 5.95, compares with the theoretical prediction value, and relative error illustrates that this scheme is reliable about 4.03%.
Embodiment 2: the method for the invention prepares the capsaicine crude extract
Get fresh chilli, wet gauze is wiped away and is put into 60 ℃ of loft drier after the surface dirt and dry to constant weight, goes handle to remove seed, stays pericarp and placenta, is ground into the powder of 40 mesh sieves with pulverizer, and it is standby to collect dry paprika.
Accurately take by weighing 0.100g capsicum powder in the volumetric flask of 10ml, add methyl alcohol to the scale marks place in volumetric flask, namely getting solid-liquid ratio is the 1:100(weightmeasurement ratio, mixture g/ml), place ultrasonic cleaner to extract capsaicine in volumetric flask, 54 ℃ of ultrasonic temperature, ultrasonic time 18min, ultrasonic power 60W, filter with quantitative paper ultrasonic intact back, collect filtrate, in filter residue and filter paper, add 10ml methyl alcohol again again, adopt same condition, be 54 ℃ of ultrasonic temperature, ultrasonic time 18min, ultrasonic power 60W, ultrasonic wave is brought up again 1 time, filter with quantitative paper, collect filtrate, collect 2 filtrates and mix, get the capsaicine extracting solution.Capsicum extract is concentrated into solid state under 0.08MPa, 50 ℃ of conditions, namely gets capsaicine crude extract A.
Comparative Examples 1: adopt the method for prior art to prepare the capsaicine crude extract
Adopt the method for people's disclosed ultrasonic extraction capsaicines in " researchs of supersound extraction capsaicine processing condition " [" modern food science and technology " 2006 the 22nd the 4th phases of volume] literary composition such as Ursidae, concrete operations are as follows:
Get fresh chilli, oven dry, dry paprika was broken into the powder of 40 mesh sieves, accurately take by weighing 2.5g capsicum powder in the volumetric flask of 50ml, add 12.5ml methyl alcohol in the volumetric flask: tetrahydrofuran (THF) (volume ratio is 1:1) supersound extraction capsaicine, 60 ℃ of ultrasonic temperature, ultrasonic time 45min, ultrasonic power 100W, filter with quantitative paper, collect filtrate, add 12.5ml methyl alcohol again in filter residue and the filter paper again: tetrahydrofuran (THF) (volume ratio is 1:1), adopt same condition, be 60 ℃ of ultrasonic temperature, ultrasonic time 45min, ultrasonic power 100W brings up again 2 times, collect 3 filtrates and mix, get the capsaicine extracting solution.Capsicum extract is concentrated into solid state under 0.08MPa, 50 ℃ of conditions, namely gets capsaicine crude extract B.
Embodiment 3: capsaicin content comparative study
Repeat embodiment 2 and Comparative Examples 1 respectively three times, obtain three different sample A1, A2, A3 and B1, B2, B3 respectively, the water content of each sample is basic identical, is approximately 5wt%.
Capsaicin content among the capsaicine detection kit method mensuration embodiment 2 that employing Beacon company provides and Comparative Examples 1 gained capsaicine crude extract A1, A2, A3 and B1, B2, the B3 repeats 3 assays experiments, averages, and the results are shown in Table 2.
The analysis of table 2 capsaicin content
By table 2 as seen, adopt the method for the invention, i.e. dry fresh chilli, go seed to remove handle, with pericarp and placenta crushing screening, get dry paprika, add organic solvent, at 54 ℃ of following supersound extraction 18min, ultrasonic power is made as 60W, extracts 2 times, filter, merging filtrate concentrates this extracting solution and gets the capsaicine crude extract, and capsaicin content is 4.55mg/g in the gained capsaicine crude extract.Compared with prior art, still make the capsaicine extraction yield improve about 10% on the basis of shortening ultrasonic time, reduction ultrasonic power greatly, greatly degree has been saved extraction cost, and has improved efficient.
In addition, adopting the measured capsaicin content variation coefficient of the inventive method is 1.10%, and the measured capsaicin content variation coefficient of prior art is 5.37%, illustrates that the inventive method extraction effect is stable, and precision is better.
Utilize method solid-liquid ratio of the present invention to be 1:100, and solid-liquid ratio only is 1:5 in the Comparative Examples 1, but organic solvent can reclaim use, so the organic solvent usage quantity greatly can be not remarkable to the increase of cost.
The above only is the preferred embodiments of the present invention, be not that the present invention is done any pro forma restriction, though the present invention discloses as above with preferred embodiment, yet be not in order to limit the present invention, any those skilled in the art, in the scope that does not break away from technical solution of the present invention, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be the content that does not break away from technical solution of the present invention, any simple modification that foundation technical spirit of the present invention is done above embodiment, equivalent variations and modification all still belong in the scope of technical solution of the present invention.

Claims (8)

1. the method for a rapid extraction capsaicine from capsicum is characterized in that, comprises the steps:
1) get fresh chilli, dust is dried to constant weight, the preparation chillies;
2) go handle to remove seed, get pericarp and the placenta of chillies;
3) crushing screening is collected dry paprika;
4) extract: get dry paprika and add the organic solvent supersound extraction, filter, get the capsaicine extracting solution;
5) aftertreatment: the capsaicine extracting solution is concentrated into solid state, namely gets the capsaicine crude extract.
2. the method for claim 1 is characterized in that, the method for preparing chillies described in the step 1) is after wet gauze is wiped clean the fresh chilli surface, to be dried to constant weight under 60 ℃.
3. method as claimed in claim 1 or 2 is characterized in that, dry paprika 100% is crossed 40 mesh sieves in the step 3).
4. the method for claim 1 is characterized in that, organic solvent described in the step 4) is methyl alcohol.
5. the method for claim 1 is characterized in that, the parameter of ultrasonic extraction process described in the step 4) is: solid-liquid ratio 1:80-1:120 (weightmeasurement ratio, g/ml), ultrasonic temperature 40-60 ℃, ultrasonic time 10-30min, ultrasonic power 60-100W, extraction time 1-2 time.
6. method as claimed in claim 5 is characterized in that, the parameter of ultrasonic extraction process described in the step 4) is: and solid-liquid ratio 1:100 (weightmeasurement ratio, g/ml), 54 ℃ of ultrasonic temperature, ultrasonic time 18min, ultrasonic power 60W, extraction time 2 times.
7. the method for claim 1 is characterized in that, the condition of the plain extracting solution of concentrated pepper described in the step 5) is: pressure 0.08MPa, 50 ℃ of temperature are concentrated into solid.
8. method as claimed in claim 7 is characterized in that, described solid water content is below the 5wt%.
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Application publication date: 20130821