JPS6339966A - Method of extracting and separating paprika orange from paprika fruit - Google Patents
Method of extracting and separating paprika orange from paprika fruitInfo
- Publication number
- JPS6339966A JPS6339966A JP61182536A JP18253686A JPS6339966A JP S6339966 A JPS6339966 A JP S6339966A JP 61182536 A JP61182536 A JP 61182536A JP 18253686 A JP18253686 A JP 18253686A JP S6339966 A JPS6339966 A JP S6339966A
- Authority
- JP
- Japan
- Prior art keywords
- paprika
- extraction
- oleoresin
- extracted
- carbon dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 240000004160 Capsicum annuum Species 0.000 title claims abstract description 56
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 title claims abstract description 56
- 239000001511 capsicum annuum Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims description 27
- 235000013399 edible fruits Nutrition 0.000 title abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 85
- 238000000926 separation method Methods 0.000 claims abstract description 66
- 239000001052 yellow pigment Substances 0.000 claims abstract description 36
- 239000000341 volatile oil Substances 0.000 claims abstract description 22
- 239000001054 red pigment Substances 0.000 claims abstract description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 90
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 45
- 239000001569 carbon dioxide Substances 0.000 claims description 45
- 239000001325 capsicum annuum l. var. longum oleoresin Substances 0.000 claims description 14
- 235000012658 paprika extract Nutrition 0.000 claims description 14
- DYUUPIKEWLHQGQ-SDXBLLFJSA-N paprika oleoresin Chemical compound C(\[C@]12[C@@](O1)(C)C[C@@H](O)CC2(C)C)=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=C[C@H]1C(C)=C[C@H](O)CC1(C)C DYUUPIKEWLHQGQ-SDXBLLFJSA-N 0.000 claims description 14
- 239000000284 extract Substances 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000008601 oleoresin Substances 0.000 description 45
- 239000003960 organic solvent Substances 0.000 description 11
- 238000002845 discoloration Methods 0.000 description 6
- 238000004508 fractional distillation Methods 0.000 description 6
- 230000009965 odorless effect Effects 0.000 description 6
- 238000004821 distillation Methods 0.000 description 5
- MCSXGCZMEPXKIW-UHFFFAOYSA-N 3-hydroxy-4-[(4-methyl-2-nitrophenyl)diazenyl]-N-(3-nitrophenyl)naphthalene-2-carboxamide Chemical group Cc1ccc(N=Nc2c(O)c(cc3ccccc23)C(=O)Nc2cccc(c2)[N+]([O-])=O)c(c1)[N+]([O-])=O MCSXGCZMEPXKIW-UHFFFAOYSA-N 0.000 description 4
- 239000002775 capsule Substances 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001058 brown pigment Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000004809 thin layer chromatography Methods 0.000 description 2
- 244000248162 Xanthoceras sorbifolium Species 0.000 description 1
- 235000009240 Xanthoceras sorbifolium Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
Description
【発明の詳細な説明】
「産業上の利用分野」
本発明は、粉砕した自然状態のパプリカ果そ（果そ＝果
更、以下同じ）から高品質の一バ灸リカオレオレジン（
以下、単にオレオレジンという）を直接抽出分離するオ
レオレジンの抽出分離方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION "Field of Industrial Application" The present invention is directed to the production of high quality one-batric moxibustion oleoresin (
The present invention relates to a method for extracting and separating oleoresin (hereinafter simply referred to as oleoresin), which directly extracts and separates oleoresin.
「従来の技術」および「発明が解決しようとする問題点
」
従来、パプリカ果そからのオレオレジンの抽出分離は、
有機溶剤による溶出抽出方法が用いられてお〕、有機溶
剤によってオレオレジンを溶出させ、その溶出したオレ
オレジンを加熱蒸留ならびに分留によって回収する方法
になっている。"Prior Art" and "Problems to be Solved by the Invention" Conventionally, the extraction and separation of oleoresin from paprika fruit was
In this method, oleoresin is eluted with an organic solvent, and the eluted oleoresin is recovered by thermal distillation and fractional distillation.
以上の従来のオレオレジンの抽出分離方法によると加熱
蒸留および分留工程が不可欠になるため、抽出分離した
オレオレジンが熱による変色によって自然の色合いを失
うと共に、有機溶剤の残留が避けられず、健康面への害
のおそれがある等の品質上の難点がある。さらに、加熱
蒸留と分留して回収したオレオレジンは、そのままでは
臭気や黄色系色素を含む為、濃紅色で無臭の良質のオレ
オレジンを得るために、複雑な脱臭工程と黄色茶色素除
去工程が必要になる問題点がある。According to the conventional extraction and separation method of oleoresin described above, heating distillation and fractional distillation steps are essential, so the extracted and separated oleoresin loses its natural color due to discoloration due to heat, and organic solvents inevitably remain. There are problems with quality, such as the possibility of harm to health. Furthermore, the oleoresin recovered through thermal distillation and fractional distillation contains odor and yellow pigments, so in order to obtain a high-quality oleoresin that is deep red and odorless, a complex deodorization process and yellow-brown pigment removal process are required. There are problems that require .
本発明は、以上の従来技術の問題点を解消し、純度の高
い高品質のオレオレジンをノ（プリカ果そからダイレク
トに抽出分離する新規の抽出分離方法を提供するのが目
的である。It is an object of the present invention to solve the problems of the above-mentioned conventional techniques and to provide a new extraction and separation method for directly extracting and separating highly pure and high quality oleoresin from fruit fruits.
「問題点を解決するための手段」
以上の目的を達成する本発明は、パプリカ果そを超臨界
状態の炭酸ガスに常温近−の温度領域で接触させ、２段
階工程の超臨界ガス抽出を行うことを技術ポイントとす
るもので、その構成要旨は「・粉砕したパプリカ果そを
抽出槽に投入して、超臨界状態の炭酸ガスと常温近傍の
温度領域で接触させ、パプリカ果そ中の精油と黄色系色
素を抽出分離すると共に、脱臭する第一抽出分離工程と
、・前記第一抽出分離工程において、精油と黄色系色素
とを抽出分離し、かう脱臭し九）（プリカ果そを、再び
常温近傍の温度領域において、超臨界状態の炭酸ガスに
接触させ、赤色系色素を抽出分離する第二抽出分離工程
、とから成るオレオレジンの抽出分離方法」が特徴であ
る。``Means for Solving the Problems'' The present invention achieves the above objectives by bringing paprika fruit into contact with carbon dioxide gas in a supercritical state at a temperature range of around room temperature, and performing a two-step supercritical gas extraction process. The technical point is to perform this process, and the gist of its composition is as follows: ・Crushed paprika fruit is placed in an extraction tank and brought into contact with carbon dioxide gas in a supercritical state at a temperature close to room temperature. A first extraction and separation step in which the essential oil and yellow pigment are extracted and separated and deodorized; - In the first extraction and separation step, the essential oil and yellow pigment are extracted and separated and deodorized. , and a second extraction and separation step in which red pigment is extracted and separated by bringing it into contact with carbon dioxide gas in a supercritical state again in a temperature region near room temperature.
詳しくは、前記の温度領域は、勲による変色変質を防止
してパプリカ果その自然状態を保持したｉま、抽出分離
することを意図したもので、前記第一、第二抽出分離工
程のいずれも、約８８℃〜５０℃の常温近傍の温度領域
を採択する。Specifically, the above-mentioned temperature range is intended to extract and separate the paprika fruit while preserving its natural state by preventing discoloration and deterioration due to oxidation, and both of the above-mentioned first and second extraction and separation steps , a temperature range near normal temperature of about 88°C to 50°C is adopted.
また、前記の超臨界状口の炭酸ガスの圧力は、前記の第
一抽出分離工程においては、パプリカ果そからの超臨界
炭酸ガスによる黄色系色素の抽出ゾーンに当る概ね１１
０ ｋｇ／ ｃｒｎ” 〜１８５ ｋｇ７ａｍ”、また
、前記の第二抽出分離工程においては、炭酸ガスの高圧
化と抽出力の向上が比例するものの、装置の耐圧性等実
用性を考慮して、概ね２００＃／Ｃ−〜ｓ ｏ Ｏ＃１
０−の圧力ゾーンを採択する。In addition, the pressure of the carbon dioxide gas at the supercritical port is approximately 11 mm, which corresponds to the extraction zone of the yellow pigment by the supercritical carbon dioxide gas from the paprika fruit in the first extraction and separation step.
0 kg/ crn" to 185 kg/7 am", and although in the second extraction and separation step, the increase in pressure of carbon dioxide gas is proportional to the improvement in extraction power, it is generally 200#/C-~so O#1
Adopt a pressure zone of 0-.
「作用」
以上の構成から成る本発明のオレオレジンの抽出分離方
法によると、前記の第一抽出分離工程においては、パプ
リカ果そが超臨界炭酸ガスによって、主として黄色系色
素のみを抽出する圧力条件において成されるため、第一
抽出分離工程において、パプリカ果そが保有する黄色系
色素と精油分が極めて有効に抽出分離されると共に、パ
プリカ果そ特有の臭気も脱臭され、その臭気は抽出され
た精油と、接触した超臨界状態の炭酸ガスに分散移転し
て放出される。"Operation" According to the oleoresin extraction and separation method of the present invention having the above-described configuration, in the first extraction and separation step, paprika fruit is exposed to supercritical carbon dioxide gas under pressure conditions such that mainly only yellow pigments are extracted. Therefore, in the first extraction and separation step, the yellow pigment and essential oil contained in paprika fruit are extracted and separated very effectively, and the odor peculiar to paprika fruit is also deodorized. It is dispersed and transferred to the supercritical carbon dioxide gas that comes into contact with the essential oil and released.
そして、前記の第二抽出分離工程では、黄色系色素と精
油を抽出分離し、かつ、脱臭したパプリカ果そを、パプ
リカ果その超臨界炭酸ガスによる赤色系色素の抽出圧力
ゾーンにおいて処理され、かつ、第一第二の抽出分離工
程のいずれもが常温近傍の温度領域で成されると共に、
有機溶剤を使用しないでダイレクト抽出されるので、処
理されるパプリカ果そは、加熱等による変色、変質の影
響を全く受けず、自然状態のままオレオレジンが抽出さ
れる。In the second extraction and separation step, the yellow pigment and essential oil are extracted and separated, and the deodorized paprika fruit is processed in a red pigment extraction pressure zone using the supercritical carbon dioxide gas of the paprika fruit. , both of the first and second extraction and separation steps are performed in a temperature range near normal temperature,
Since it is directly extracted without using organic solvents, the processed paprika fruit is not affected by discoloration or deterioration due to heating, etc., and oleoresin is extracted in its natural state.
従って、本発明のオレオレジンの抽出分離方法によると
、残存有機溶剤のおそれがなく、無臭にして自然のまま
であシ、極めて色価の高い高品位高品質のオレオレジン
を抽出分離することかで蕪る。Therefore, according to the oleoresin extraction and separation method of the present invention, it is possible to extract and separate a high-grade, high-quality oleoresin that is odorless, natural, and has an extremely high color value without the risk of residual organic solvents. Soak it.
「実施例」
以下、実施例を引用して詳しく説明する。その一実施例
の抽出装置を示す第１図を参照して、本発明のオレオレ
ジンの抽出分離は、会知の超臨界ガス抽出分離装置を用
いて行うもので、抽出ガスとして炭酸ガスを用い、以下
の手順によってオレオレジンを精製する。"Example" Hereinafter, a detailed explanation will be given with reference to an example. Referring to FIG. 1 showing an example of an extraction apparatus, the extraction and separation of oleoresin of the present invention is carried out using a well-known supercritical gas extraction and separation apparatus, using carbon dioxide gas as the extraction gas. , the oleoresin is purified by the following procedure.
（１）第一抽出分離工程
粉砕したパプリカ果そ８．５２１を、容量２Ｑａｃのス
テンレス製円筒体の抽出槽１に投入し、抽出槽１を４０
℃に保持しながら、加圧した炭酸ガスを導入して抽出槽
１の内圧を１８５ ｋｇ／ ａｍ”に昇圧し、約６０分
間保持して、投入したパプリカ果そと超臨界状態の炭酸
ガスとを接触させる。(1) First extraction and separation step 8.521 of the crushed paprika fruits are put into the stainless steel cylindrical extraction tank 1 with a capacity of 2Qac.
While maintaining the temperature at °C, pressurized carbon dioxide gas was introduced to raise the internal pressure of extraction tank 1 to 185 kg/am'', and the mixture was held for approximately 60 minutes to combine the added paprika and carbon dioxide gas in a supercritical state. contact.
続いて、抽出槽１内の抽出物を分離槽２に移し、炭酸ガ
スを気化させて減圧し、分離槽２の下部にパプリカ果そ
から抽出した精油と黄色千色素を抽出分離すると共に、
パプリカ果そ特有の臭気を脱臭させた。なお、分離槽２
の下部から取シ出した精油と黄色系色素の合計は０．０
４．Ｉである。Next, the extract in the extraction tank 1 is transferred to the separation tank 2, the carbon dioxide gas is vaporized and the pressure is reduced, and the essential oil extracted from the paprika fruit and the yellow pigment are extracted and separated in the lower part of the separation tank 2.
Deodorizes the characteristic odor of paprika fruit. In addition, separation tank 2
The total amount of essential oil and yellow pigment taken out from the bottom of is 0.0
4. It is I.
（２）第二抽出分離工程
つぎに、抽出槽１を４０℃に保持しながら再び炭酸ガス
を導入し、抽出槽１の内圧を５００ｋｆ’ ｃｒｎ”に
昇圧して約６０分間保持し、前記の第一抽出分離工程に
よって精油と黄色系色素とを抽出分離すると共に、脱臭
したパプリカ果そと超臨界状態の炭酸ガスとを再び接触
させて赤色系色素を抽出した。(2) Second extraction and separation step Next, while maintaining the extraction tank 1 at 40°C, carbon dioxide gas is introduced again, and the internal pressure of the extraction tank 1 is increased to 500 kf'crn'' and held for about 60 minutes. In the first extraction and separation step, the essential oil and the yellow pigment were extracted and separated, and the deodorized paprika pulp was brought into contact with carbon dioxide gas in a supercritical state again to extract the red pigment.
続いて、抽出された赤色系色素を分離槽２へ移して炭酸
ガスを気化させ、分離槽２の下部に濃紅色にしてペース
ト状のオレオレジンを０．１７１ｉ１出分離した。Subsequently, the extracted red pigment was transferred to the separation tank 2 to vaporize the carbon dioxide gas, and 0.171 l of oleoresin in the form of a deep red paste was separated at the bottom of the separation tank 2.
なお、前記の第一抽出分離工程において、抽出分離した
精油と、気化放散した炭酸ガスが、パプリカ果そ特有の
臭気を強く帯有し、抽出槽１内のパプリカ果そが充分に
脱臭されたことを確認した。In addition, in the first extraction and separation step, the extracted and separated essential oil and the vaporized carbon dioxide gas had a strong odor peculiar to paprika fruits, and the paprika fruits in the extraction tank 1 were sufficiently deodorized. It was confirmed.
以上の実施例のプロセスによって抽出分離されたオレオ
レジンを、色差計によって測定し、従来手段によるオレ
オレジンと対比した結果は、下記第一表の通シであシ（
参考図表（イ）参照）、本発明の抽出分離方法によるパ
プリカオレオレジンは、Ｃ，Ｖ、（色価）＝２４４，７
２８、ｂ／ａ ＝ ４．２２５を示し、極めて赤色度が
高く高品質のパプリカオレオレジンであることを明白に
した。The oleoresin extracted and separated by the process of the above example was measured with a color difference meter and compared with the oleoresin produced by conventional means.The results are shown in Table 1 below.
Refer to reference diagram (a)), the paprika oleoresin obtained by the extraction separation method of the present invention has C, V, (color value) = 244,7
28, b/a = 4.225, making it clear that the paprika oleoresin had an extremely high degree of redness and was of high quality.
第一表
なお、本発明の前記の第一抽出分離工程において、超臨
界炭酸ガス圧力と抽出される黄色系色素との相関は、薄
層クロマトグツフィー法によって測定した結果（参考図
表向参照）、炭酸ガス圧力が概ね１１０ ｋｇ／６−〜
１８０１ｇ／ｃ−のゾーンにおいては、黄色系色素のみ
が抽出されるものの、概ね１４０ ＃／ ａｍ〜１６０
＃／ａｍの圧力ゾーンにおいて、赤色系色素と共に微
量の黄色系色素が抽出される（圧力の向上に比例して赤
色系色素の抽出量が増加し、黄色系色素の抽出量が漸減
する）特性がある。Table 1 In addition, in the first extraction and separation step of the present invention, the correlation between the supercritical carbon dioxide gas pressure and the yellow pigment extracted is the result of measurement by thin layer chromatography method (see reference figure direction) , carbon dioxide pressure is approximately 110 kg/6-~
In the 1801 g/c- zone, only yellow pigment is extracted, but it is generally 140 #/am to 160
In the pressure zone of #/am, a trace amount of yellow pigment is extracted along with the red pigment (the amount of red pigment extracted increases in proportion to the increase in pressure, and the amount of yellow pigment extracted gradually decreases). There is.
従って、以上の相関特性から、実用的にオレオレジンを
量産する経済性を考慮して、前記の実施例では第一抽出
分離工程の炭酸ガス圧力を１８５１ｇ／ａｍ”に採択し
て黄色系色素をｉ山分離し、Ｃ０Ｖ。Therefore, in consideration of the economic efficiency of mass-producing oleoresin from the above correlation characteristics, in the above example, the carbon dioxide pressure in the first extraction and separation step was adopted as 1851 g/am'' to produce a yellow pigment. i mountain separated and C0V.
＝２４４，７２８のオレオレジンを抽出分離した。=244,728 oleoresins were extracted and separated.
しかし、抽出分離して生成するパプリカオレオレジンの
歩留（最初に投入したパプリカ果そに対するパプリカオ
レオレジンの抽出分離量の割合）を犠牲にして、第一抽
出分離工程における炭酸ガス圧力を、例えば１６０ ｋ
４７ｅｍ程度に上昇させ、赤色系色素と共に抽出される
黄色系色素を充分に抽出□分離させると、□第二抽出分
離工程によって、例えばＣ，Ｖ、＝２６０，０００の極
限状態の超高品位のパプリカオレオレジンを抽出分離す
るヒとが技術的に可能である。However, at the expense of the yield of paprika oleoresin produced by extraction and separation (the ratio of the amount of paprika oleoresin extracted and separated to the initially charged paprika fruit), the carbon dioxide pressure in the first extraction and separation step is reduced, for example. 160k
When the yellow pigment extracted together with the red pigment is sufficiently extracted and separated, the second extraction and separation process produces ultra-high-quality ultra-high-grade pigments in the extreme state of, for example, C, V = 260,000. It is technically possible to extract and separate paprika oleoresin.
「発明の効果」
以上の説明の様に、本発明のオレオレジンの抽出分離方
法は、温度と圧力の制御による簡便な２段階プロセスの
超臨界炭酸ガス抽出によって、無臭くして、有機溶剤等
を含まない自然状口であシ、かつ色価が２４万を超える
高品位高品質のパプリカオレオレジンを連続的に抽出生
成するｗ４著な効果がある。"Effects of the Invention" As explained above, the method for extracting and separating oleoresins of the present invention uses supercritical carbon dioxide gas extraction, a simple two-step process by controlling temperature and pressure, to make the oleoresin odorless and free from organic solvents. W4 has the remarkable effect of continuously extracting and producing high-grade, high-quality paprika oleoresin with a natural taste and a color value exceeding 240,000.
第１図工本発明−実施例に用いた抽出分離装置の概念図
符号、１：抽出槽、２：分離槽、８：炭酸ガスボンベ、
４：コンプレ、サー、５：圧力制御弁特許出願人
茂利製油株式会社代理人弁理士
岡 賢 美手続補正書
昭和６２年 １月２ｂ日
昭和６１年特 許 願第１８Ｌ１５８６号事件との関係
特許出願人
６、 補正により増加する発明の数 Ｏ別
紙
「明細書の発明の詳細な説明の欄」を以下の通シ全文補
正する（即ち、全文中に訃ける「果そ」を、すべて「果
きょう」と補正するン。
「８１発明の詳細な説明
「産業上の利用分野」
本発明は、粉砕した自然状態のパプリカ果きよう（果き
ょう＝果莢、以下同じ）から高品質のパプリカオレオレ
ジン（以下、単にオレオレジンという）を直接抽出分離
するオレオレジンの抽出分離方法に関するものである。
「従来の技術」および「発明が解決しようとする問題点
」
従来、パプリカ果きょうからのオレオレジンの抽出分離
は、有機溶剤による溶出抽出方法が用いられておシ、有
機溶剤によってオレオレジンを溶出させ、その溶出した
オレオレジンを加熱蒸留ならびに分留によって回収する
方法になっている。
以上の従来のオレオレジンの抽出分離方法によると加熱
蒸留および分留工程が不可欠になる丸め、抽出分離し九
オレオＶジンが熱による変色によって自然の色合いを失
うと共に、有機溶剤の残留が避けられず、健康面への害
のおそれがある岬の品質上の難点がある。さらに、加熱
蒸留と分留して回収し九オＶオレジンは、そのｔまでは
臭気や黄色系色素を含む為、濃紅色で無臭の良質のオレ
オレジンを得るために、複雑な脱臭工程と黄色系色素除
去工程が必要になる問題点がある。
本発明は、以上の従来技術の問題点を解消し、純度の高
い高品質のオレオレジンをパプリカ果きょうからダイレ
フ）Ｋ抽出分離する新規の抽出分離方法を提供するのが
目的である。
「問題点を解決するための手段」
以上の目的を達成する本発明は、パプリカ果きょうを超
臨界状態の炭酸ガスに常温近傍の温度領域で接触させ、
２段階工程の超臨界ガス抽出を行うことを技術ポイント
とするもので、その構成要旨は
「・粉砕したパプリカ果きょうを抽出槽に投入して、超
臨界状態の炭酸ガスと常温近傍の温度領域で接触させ、
パプリカ果きょう中の精油と黄色系色素を抽出分離すゐ
と共に、脱臭する第一抽出分離工程と、
・前記第一抽出分離工程において、精油と黄色系色素と
を抽出分離し、かつ脱臭したパプリカ果きょうを、再び
常温近傍の温度領域において、超臨界状態の炭酸ガスに
接触させ、赤色系色素を抽出分離する第二抽出分離工程
、とから成るオレオレジンの抽出分離方法」が特徴であ
る。
詳しくは、前記の温度領域は、熱による変色変質を防止
してパプリカ果きょうの自然状態を保持したｔま、抽出
分離することを意図したもので、前記第一、第二抽出分
離工程のいずれも、約８８℃〜５０℃の常温近傍の温度
領域を採択する。
また、前記の超臨界状態の炭酸ガスの圧力は、前記の第
一抽出分離工程においては、パプリカ果きょうからの超
臨界炭酸ガスによる黄色系色素の抽出ゾーンに当る概ね
１１０ ＃１０１ｎ” 〜１８５＃１０ｊ。
また、前記の第二抽山分は工程においては、炭酸ガスの
高圧化と抽出力の向上が比例するものの、装置の耐圧性
等実用性を考慮して、概ね２００ｋｇ／ ａｍ”〜５
Ｇ Ｇ ｋｇｌｏ−の圧力ゾーンを採択する。
「作用」
以上の構成から成る本発明のオレオレジンの抽出分離方
法によると、前記の第一抽出分離工程においては、パプ
リカ果きょうが超臨界炭酸ガスによって、主として黄色
系色素のみを抽出する圧力条件において成されるため、
第一抽出分離工程において、パプリカ果きょうが保有す
る黄色系色素と精油分が極めて有効に抽出分離されると
共に、パプリカ果きょう特有の臭気も脱臭され、その臭
気は抽出された精油と、接触した超臨界状態の炭酸ガス
に分散移転して放出される。
そして、前記の第二抽出分離工程では、黄色系色素と精
油を抽出分離し、かつ、脱臭したパプリカ果きょうを、
パプリカ果きょうの超臨界炭酸ガスによる赤色系色素の
”ｉ出圧カゾーンにおいて処理され、かつ、第一第二の
抽出分離工程のいずれもが常温近傍の温度領域で成され
ると共に、有機溶剤を使用しないでダイレクト抽出され
るので、処理されるパプリカ果きょうは、加熱等による
変色、変質の影響を全く受けず、自然状態の１１オＶオ
レジンが抽出される。
従って、本発明のオレオレジンの抽出分離方法によると
、残存有機溶剤のおそれがなく、無臭にして自然のまま
であシ、極めて色価の高い高品位高品質のオレオレジン
を抽出分離することができる。
「実施例」
以下、実施例を引用して詳しく説明する。その一実施例
の抽出装置を示す第１図を参照して、本発明のオレオレ
ジンの抽出分離は、公知の超臨界ガス抽出分離装置を用
いて行うもので、抽出ガスとして炭酸ガスを用い、以下
の手順によってオレオレジンを精製する。
（１）第一抽出分離工程
粉砕したパプリカ果きょう８．５２ｆを、容量２０ａｃ
のステンレス製円筒体の抽出槽１に投入し、抽出槽１を
４０℃に保持しながら、加圧した炭酸ガスを導入して抽
出Ｍ１１の内圧を１８５９／ａｍ”Ｋ昇圧し、約６０分
間保持して、投入したパプリカ来電ようと超臨界状態の
炭酸ガスとを接触させる。
続いて、抽出槽ｌ内の抽出物を分離槽２に移し、炭酸ガ
スを気化させて減圧し、分離槽２の下部にパプリカ果き
ょうから抽出し九精油と黄角系色素を抽出分離すると共
に、パプリカ果きょう特有の臭気を脱臭させた。なお、
分離槽２の下部から取シ出した精油と黄色系色素の合計
は０．０４Ｆである。
（２）第二抽出分離工程
つぎに、抽出槽１を４０℃に保持しながら再び炭酸ガス
を導入し、抽出槽ｌの内圧を５００＃／ｃＴＩ！に外圧
して約６０分間保持し、前記の第一抽出分離工程によっ
て精油と黄色系色素とを抽出分離すると共に、脱臭した
パプリカ果きょうと超臨界状態の炭酸ガスとを再び接触
させて赤色系色素を抽出した。
続いて、抽出された赤色系色素を分離槽２へ移して炭酸
ガスを気化させ、分離槽２の下部に濃紅色にしてペース
ト状のオレオレジンを０．１７１抽出分離した。
なお、前記の第一抽出分離工程において、抽出分離した
精油と、気化放散した炭酸ガスが、パプリカ果きょう特
有の臭気を強く帯有し、抽出ｍｌ内のパプリカ果きょう
が充分に脱臭されたことを確認した。
以上の実施例のプロセスによって抽出分離されたオレオ
レジンを、色差計によって測定し、従来手段によるオレ
オレジンと対比した結果は、下記第一表の通シであ）（
参考図表に）参照）、本発明の抽出分離方法によるパプ
リカオレオレジンは、Ｃ，Ｖ、（色価）＝２４４．７！
８、ｂ／ａ−４，２２５を示し、極めて赤色度が高く高
品質のパプリカオレオレジンであることを明白にした。
なお１本発明の前記の第一抽出分離工程において、超臨
界炭酸ガス圧力と抽出される黄色系色素との相関は、薄
層クロマトグツフィー法によって測定した結果（参考図
表向参照）、炭酸ガス圧力が概ね１１０ ＃、１０ｄ〜
１８０ ｋｆ／ｃｔｒｌのゾーンにおいては、黄色系色
素のみが抽出されるものの、概ね１４０ ｋｇ／ ｃｍ
１〜１６０ ＃／Ｃ−の圧力ゾーンにおいて、赤色系色
素と共に微量の黄色系色素が抽出される（圧力の向上に
比例して赤色系色素の抽出量が増加し、黄色系色素の抽
出量が漸減する）特性がある。
従って、以上の相関特性から、実用的にオレオレジンを
量産する経済性を考慮して、前記の実施例では第一抽出
分離工程の炭酸ガス圧力を１３６ｋｇ／ａｍ”に採択し
て簀色系色素を抽出分離し、Ｃ，Ｖ。
”’２４４，７２８のオレオレジンを抽出分離した。
しかし、抽出分離して生成するパプリカオレオレジンの
歩留（最初に投入したパプリカ果きょうに対するパプリ
カオレオレジンの抽出分離景の割合）を犠牲にして、第
一抽出分離工程における炭酸ガス圧力を、例えば１６０
１ｇ／ａｍ”程度に上昇させ、赤色系色素と共に抽出さ
れる黄色系色素を充分に抽出分離させると、第二抽出分
離工程によって、例えばＣ０■、＝２６０．０００の極
限状態の超高品位のパプリカオレオレジンを抽出分離す
ることが技術的に可能である。
「発明の効果」
以上の説明の様に、本発明のオレオレジンの抽出分離方
法は、温度と圧力の制御による簡便な２段階プロセスの
超臨界炭酸ガス抽出によって、無臭にして、有機溶剤等
を含まない自然状態であシ、かつ色価が２４万を超える
高品位高品質のバデリ。
カオレオレジンを連続的に抽出生成する顕著な効果があ
る。」Fig. 1 Conceptual diagram of the extraction and separation apparatus used in the present invention-examples Codes: 1: extraction tank, 2: separation tank, 8: carbon dioxide cylinder,
4: Compressor, sir, 5: Pressure control valve patent applicant
Patent attorney representing Shigeru Oil Co., Ltd.
Kenbi Oka Procedural Amendment Letter January 2b, 1985 Relationship with Patent Application No. 18L1586 of 1986 Patent Applicant 6, Number of Inventions Increased by Amendment by O
The entire text of the paper ``Detailed explanation of the invention in the specification column'' is amended as follows (i.e., all ``Kaso'' in the entire text are amended to ``Kakyo''. ``81 Details of the invention.'' Description "Industrial Application Field" The present invention is a method for directly extracting high-quality paprika oleoresin (hereinafter simply referred to as oleoresin) from crushed paprika fruit pods (the same applies hereinafter) in their natural state. The present invention relates to a method for extracting and separating oleoresin to be separated. "Prior art" and "problems to be solved by the invention" Conventionally, oleoresin was extracted and separated from paprika fruit by an elution extraction method using an organic solvent. In this method, the oleoresin is eluted with an organic solvent, and the eluted oleoresin is recovered by thermal distillation and fractional distillation. Due to the quality of the cape, the fractional distillation process is essential, and nine oleo-V gins lose their natural color due to discoloration due to heat, and residual organic solvents are unavoidable, which may be harmful to health. In addition, the nine-o-V oleoresin that is recovered by thermal distillation and fractional distillation contains odor and yellow pigments up to that point, so in order to obtain a high-quality oleoresin that is deep red and odorless, a complex process is required. There is a problem that a deodorizing process and a yellow pigment removal process are required.The present invention solves the problems of the above-mentioned conventional technology and extracts highly pure and high quality oleoresin from paprika pods. The purpose is to provide a novel extraction and separation method for separation. "Means for Solving the Problems" The present invention achieves the above objects by bringing paprika pods into contact with carbon dioxide gas in a supercritical state at a temperature around room temperature,
The technical point is to perform supercritical gas extraction in a two-step process. make contact with
A first extraction and separation step in which the essential oil and yellow pigment in the paprika fruit pods are extracted and separated, as well as deodorized; - In the first extraction and separation step, the essential oil and yellow pigment are extracted and separated, and the deodorized paprika A method for extracting and separating oleoresins is characterized by a second extraction and separation step in which the fruit pods are brought into contact with carbon dioxide gas in a supercritical state again at a temperature around room temperature to extract and separate the red pigment. Specifically, the above-mentioned temperature range is intended to perform extraction and separation while preserving the natural state of the paprika pods by preventing discoloration and deterioration due to heat. Also, a temperature range of about 88° C. to 50° C. near normal temperature is adopted. In addition, the pressure of the carbon dioxide gas in the supercritical state is approximately 110 #101n'' to 185 #1, which corresponds to the extraction zone of the yellow pigment by the supercritical carbon dioxide gas from the paprika fruit in the first extraction and separation step. 10j. In addition, although the above-mentioned second extraction amount is proportional to the increase in pressure of carbon dioxide gas and the improvement in extraction power in the process, it is approximately 200 kg/am" to 5
Adopt a pressure zone of G G kglo-. "Operation" According to the oleoresin extraction and separation method of the present invention having the above-mentioned configuration, in the first extraction and separation step, paprika pods are exposed to supercritical carbon dioxide gas under pressure conditions such that mainly only yellow pigments are extracted. Because it is done in
In the first extraction and separation step, the yellow pigment and essential oil contained in the paprika fruit are extracted and separated very effectively, and the odor peculiar to the paprika fruit is also deodorized. It is dispersed and transferred to carbon dioxide gas in a supercritical state and released. In the second extraction and separation step, the yellow pigment and essential oil are extracted and separated, and the deodorized paprika fruit is
The paprika pods are treated in a pressure zone where red pigments are extracted using supercritical carbon dioxide gas, and both the first and second extraction and separation steps are performed in a temperature range near room temperature, and organic solvents are not used. Since the oleoresin of the present invention is directly extracted without using it, the processed paprika is not affected by discoloration or deterioration due to heating etc., and the 11V oleoresin in its natural state is extracted. According to the extraction separation method, it is possible to extract and separate a high-grade, high-quality oleoresin that is odorless and natural without the risk of residual organic solvents and has an extremely high color value. This will be explained in detail by citing examples. Referring to FIG. 1 showing an example of an extraction apparatus, the extraction and separation of oleoresin of the present invention is carried out using a known supercritical gas extraction and separation apparatus, using carbon dioxide gas as the extraction gas, The oleoresin is purified by the following procedure. (1) First extraction and separation step 8.52f of crushed paprika fruit is added to a capacity of 20ac.
The internal pressure of the extraction M11 was increased to 1859/am"K by introducing pressurized carbon dioxide while maintaining the extraction tank 1 at 40°C, and held for about 60 minutes. Then, the introduced paprika is brought into contact with carbon dioxide gas in a supercritical state.Next, the extract in extraction tank 1 is transferred to separation tank 2, and the carbon dioxide gas is vaporized and depressurized. In the lower part of the paprika capsule, nine essential oils and yellow horn pigments were extracted and separated, and the odor peculiar to paprika capsules was deodorized.
The total amount of essential oil and yellow pigment taken out from the bottom of separation tank 2 is 0.04F. (2) Second extraction and separation step Next, while maintaining the extraction tank 1 at 40°C, carbon dioxide gas is introduced again, and the internal pressure of the extraction tank 1 is set to 500#/cTI! External pressure is maintained for about 60 minutes, and the essential oil and yellow pigment are extracted and separated in the first extraction and separation step, and the deodorized paprika pods are brought into contact with carbon dioxide gas in a supercritical state again to obtain the red pigment. was extracted. Subsequently, the extracted red pigment was transferred to separation tank 2 to vaporize the carbon dioxide gas, and 0.171 of a paste-like oleoresin was extracted and separated at the bottom of separation tank 2 in a deep red color. In addition, in the first extraction and separation step, the extracted and separated essential oil and the vaporized carbon dioxide gas had a strong odor peculiar to paprika capsules, and the paprika capsules in the extracted ml were sufficiently deodorized. It was confirmed. The oleoresin extracted and separated by the process of the above example was measured with a colorimeter and compared with the oleoresin produced by conventional means.The results are shown in Table 1 below.
(Refer to the reference chart), the paprika oleoresin obtained by the extraction separation method of the present invention has C, V, (color value) = 244.7!
8, b/a-4,225, clearly indicating that it was a high quality paprika oleoresin with extremely high redness. 1. In the first extraction and separation step of the present invention, the correlation between the supercritical carbon dioxide pressure and the extracted yellow pigment was determined by the thin layer chromatography method (see the reference figure). Pressure is approximately 110#, 10d~
In the 180 kf/ctrl zone, only yellow pigments are extracted, but approximately 140 kg/cm
In the pressure zone of 1 to 160 #/C-, a small amount of yellow pigment is extracted together with red pigment (the amount of red pigment extracted increases in proportion to the increase in pressure, and the amount of yellow pigment extracted increases). It has the characteristic of gradually decreasing. Therefore, from the above-mentioned correlation characteristics, and considering the economic efficiency of mass-producing oleoresin, in the above example, the carbon dioxide pressure in the first extraction and separation step was adopted as 136 kg/am'' to produce a dark brown pigment. was extracted and separated, and the oleoresin of C, V.'''244,728 was extracted and separated. However, at the expense of the yield of paprika oleoresin produced by extraction and separation (the ratio of the extracted and separated amount of paprika oleoresin to the initially charged paprika canes), the carbon dioxide pressure in the first extraction and separation step is reduced, for example. 160
1 g/am" and sufficiently extract and separate the yellow pigment extracted together with the red pigment. In the second extraction and separation process, an ultra-high quality product with an extreme condition of C0, = 260,000, for example, is produced. It is technically possible to extract and separate paprika oleoresin. "Effects of the Invention" As explained above, the method for extracting and separating paprika oleoresin of the present invention is a simple two-step process by controlling temperature and pressure. This is a high-grade, high-quality Baddeli that is made odorless through supercritical carbon dioxide gas extraction, remains in its natural state without any organic solvents, etc., and has a color value of over 240,000. It has a remarkable effect of continuously extracting and producing kaoleoresin. ”
Claims (1)
臨界状態の炭酸ガスと常温近傍の温度領域において接触
させ、パプリカ果莢中の精油と黄色系色素を抽出分離す
ると共に、脱臭する第一抽出分離工程と、 ・前記第一抽出分離工程において、精油と黄色系色素と
を抽出分離し、かつ脱臭したパプリカ果莢を、再び常温
近傍の温度領域において、超臨界状態の炭酸ガスに接触
させ、赤色系色素を抽出分離する第二抽出分離工程、 とから成ることを特徴とするパプリカ果莢からのパプリ
カオレオレジンの抽出分離方法。(1) The crushed paprika pods are placed in an extraction tank and brought into contact with supercritical carbon dioxide gas at a temperature close to room temperature to extract and separate the essential oil and yellow pigment in the paprika pods, as well as deodorize them. - In the first extraction and separation step, the essential oil and the yellow pigment have been extracted and separated, and the deodorized paprika pods are heated again in a temperature region near room temperature to carbon dioxide gas in a supercritical state. A method for extracting and separating paprika oleoresin from paprika pods, comprising: a second extraction and separation step of contacting the paprika pods with extracting and separating a red pigment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61182536A JPS6339966A (en) | 1986-08-01 | 1986-08-01 | Method of extracting and separating paprika orange from paprika fruit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61182536A JPS6339966A (en) | 1986-08-01 | 1986-08-01 | Method of extracting and separating paprika orange from paprika fruit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6339966A true JPS6339966A (en) | 1988-02-20 |
Family
ID=16120017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61182536A Pending JPS6339966A (en) | 1986-08-01 | 1986-08-01 | Method of extracting and separating paprika orange from paprika fruit |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6339966A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5207841A (en) * | 1990-04-12 | 1993-05-04 | Tdk Corporation | Soft magnetic powder and magnetic shield composition |
| US7815958B2 (en) | 2001-06-14 | 2010-10-19 | San-Ei Gen F.F.I., Inc. | Carotenoids color emulsion preparation |
| CN102321384A (en) * | 2011-06-21 | 2012-01-18 | 西北大学 | Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method |
| CN102433020A (en) * | 2011-12-21 | 2012-05-02 | 晨光生物科技集团股份有限公司 | Method for preparing natural brown pigment from cotton seed |
| CN102757665A (en) * | 2012-07-28 | 2012-10-31 | 吉林省金塔实业（集团）股份有限公司 | Degumming process of capsicum extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61268762A (en) * | 1985-05-24 | 1986-11-28 | Mitsubishi Kakoki Kaisha Ltd | Concentration of naturally-occurring dyestuff |
-
1986
- 1986-08-01 JP JP61182536A patent/JPS6339966A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61268762A (en) * | 1985-05-24 | 1986-11-28 | Mitsubishi Kakoki Kaisha Ltd | Concentration of naturally-occurring dyestuff |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5207841A (en) * | 1990-04-12 | 1993-05-04 | Tdk Corporation | Soft magnetic powder and magnetic shield composition |
| US7815958B2 (en) | 2001-06-14 | 2010-10-19 | San-Ei Gen F.F.I., Inc. | Carotenoids color emulsion preparation |
| CN102321384A (en) * | 2011-06-21 | 2012-01-18 | 西北大学 | Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method |
| CN102433020A (en) * | 2011-12-21 | 2012-05-02 | 晨光生物科技集团股份有限公司 | Method for preparing natural brown pigment from cotton seed |
| CN102757665A (en) * | 2012-07-28 | 2012-10-31 | 吉林省金塔实业（集团）股份有限公司 | Degumming process of capsicum extract |
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