JPH0643445B2 - Pectin manufacturing method - Google Patents

Pectin manufacturing method

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Publication number
JPH0643445B2
JPH0643445B2 JP58238916A JP23891683A JPH0643445B2 JP H0643445 B2 JPH0643445 B2 JP H0643445B2 JP 58238916 A JP58238916 A JP 58238916A JP 23891683 A JP23891683 A JP 23891683A JP H0643445 B2 JPH0643445 B2 JP H0643445B2
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JP
Japan
Prior art keywords
pectin
extract
concentration
insoluble matter
separated
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.)
Expired - Lifetime
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Japanese (ja)
Other versions
JPS60133002A (en
Inventor
晶二 鈴木
弘文 二宮
卓 田渕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Acetate Co Ltd
Mitsubishi Rayon Co Ltd
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Mitsubishi Acetate Co Ltd
Mitsubishi Rayon Co Ltd
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Priority to JP58238916A priority Critical patent/JPH0643445B2/en
Publication of JPS60133002A publication Critical patent/JPS60133002A/en
Publication of JPH0643445B2 publication Critical patent/JPH0643445B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Jellies, Jams, And Syrups (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

【発明の詳細な説明】 本発明はペクチンの製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing pectin.

ペクチンは、細胞間の充填並びに組織の支持に役立つ物
質として、植物界一般に広く分布しているコロイド状の
細胞壁多糖類であつて、主としてD−ガラクツロン酸の
α−1,4結合より構成され、アラビノース、ガラクトー
ス、ラムノース等の中性糖を種々の割合で含有してい
る。特にレモン、ライム、オレンジ、グレープフルーツ
等の柑橘類の果皮、リンゴ等には良質のペクチンが相当
量含まれ、欧米諸国ではこれらを原料としてペクチンの
製造がなされている。ペクチン分子中のD−ガラクツロ
ン酸のカルボキシル基は部分的にメチルエステル化され
ており、メトキシル化度50%以上のものはハイメトキ
シル(HM)ペクチン、50%以下のものはロウメトキシ
ル(LM)ペクチンと分類される。これらはそれぞれゲル
化の機構やゲル化条件が異なつているが、ペクチンが低
pH系で安定なゲルを形成するという性質、並びに低pH系
で保護コロイド的な働きをするという性質を利用して、
ジヤム、ママレード、ゼリー菓子、果汁飲料、ヨーグル
ト等として食品業界で広く利用されている。
Pectin is a colloidal cell wall polysaccharide widely distributed in the plant kingdom and is mainly composed of α-1,4 bond of D-galacturonic acid as a substance useful for filling cells and supporting tissues. It contains neutral sugars such as arabinose, galactose and rhamnose in various proportions. Particularly, citrus peels such as lemons, limes, oranges, and grapefruits, apples, and the like contain a large amount of high-quality pectin, and pectin is produced using these as a raw material in Western countries. The carboxyl group of D-galacturonic acid in the pectin molecule is partially methyl-esterified. High methoxyl (HM) pectins with a methoxylation degree of 50% or more, and low methoxyl (LM) pectins with a methoxylation degree of 50% or less. Is classified as. These have different gelation mechanisms and gelation conditions, but their pectin levels are low.
Utilizing the property of forming a stable gel in the pH system and the property of acting as a protective colloid in the low pH system,
It is widely used in the food industry as a jam, marmalade, jelly confectionery, fruit juice drink, yogurt, etc.

柑橘類果皮等よりペクチンを製造する一般的な方法は次
のとおりである。果皮を冷水又は/及び温水で数回洗浄
し、果皮中の糖、有機酸、色素等の水溶性物質を除去
し、次いで塩酸、硫酸等の無機酸でペクチンを加熱抽出
する。この抽出液を遠心分離、圧搾分離等により不溶解
分を分離し、分離液に珪藻土等の過助剤を添加し清澄
過を行う。得られた過液を濃縮してメタノール、イ
ソプロピルアルコール、アセトン等の水混和性有機溶剤
を加えるか、あるいはアルミニウム、銅、鉄等の金属の
塩を添加してペクチンを該金属塩として沈殿させ、脱水
回収する。金属塩法による場合は続いて酸性アルコール
等で沈殿を洗浄し、金属分を除去して可溶化させる必要
がある。いずれの場合でも、ペクチンの沈殿を乾燥、粉
砕して粉末ペクチンとする。
The general method for producing pectin from citrus peel and the like is as follows. The pericarp is washed several times with cold water and / or warm water to remove water-soluble substances such as sugar, organic acid and pigment in the pericarp, and then pectin is heated and extracted with an inorganic acid such as hydrochloric acid and sulfuric acid. Insoluble matter is separated from this extract by centrifugation, compression separation, etc., and a super-auxiliary agent such as diatomaceous earth is added to the separated solution for clarification. The resulting excess liquid is concentrated to add a water-miscible organic solvent such as methanol, isopropyl alcohol, or acetone, or a metal salt such as aluminum, copper, or iron is added to precipitate pectin as the metal salt, Dehydrate and collect. In the case of the metal salt method, it is necessary to subsequently wash the precipitate with acidic alcohol or the like to remove the metal content and solubilize it. In either case, the pectin precipitate is dried and ground into powder pectin.

このような一般的なペクチンの製造方法における最大の
問題点は、ペクチンの抽出濃度の低さである。乾燥した
ペクチン原料果皮中に含まれるペクチンの割合は原料の
種類、産地、収穫時期等により一定でないが、ほぼ10
〜20%程度と言われており、抽出を行つた場合、ペク
チン分よりも不溶解の残査部分の方が圧倒的に多い状況
にある。不溶解残査の分離方法として例えば遠心分離を
利用する場合は、分離された残査の固形分濃度が低いた
めに、抽出液の濃度を高くすればするほど分離液の収率
が低下する。例えば抽出液濃度が1%の場合には該分離
液の収率が75%程度であるのに対し、濃度が1.5%程
度になると分離液の収率は50%程度に低下し、かえつ
て不利な結果を招く。圧搾法により残査分離を行う場合
には、不溶解分が極めて軟質であるため、すべりが生じ
て十分な圧搾ができず、残査の固形分濃度も上がらず、
スクリーンの目詰まり等を起こしやすい。
The biggest problem in such a general pectin production method is the low extraction concentration of pectin. The ratio of pectin contained in dried pectin raw material peels is not constant depending on the type of raw material, production area, harvest time, etc.
It is said to be about 20%, and when extraction is performed, the undissolved residual portion is overwhelmingly larger than the pectin content. When, for example, centrifugation is used as a method for separating the undissolved residue, the solid content concentration of the separated residue is low, and thus the higher the concentration of the extract, the lower the yield of the separated solution. For example, when the concentration of the extract is 1%, the yield of the separated liquid is about 75%, whereas when the concentration is about 1.5%, the yield of the separated liquid is reduced to about 50%, which is disadvantageous. With unpredictable results. When the residual separation is carried out by the compression method, the insoluble content is extremely soft, slippage occurs, sufficient compression cannot be performed, and the solid content concentration of the residual does not increase,
The screen is easily clogged.

かかる事情により従来行われているペクチンの製造方法
によれば、ペクチンの濃度限界はせいぜい1%であり、
これより高い場合には不溶解残査分離の困難さから、か
えつて効率が低下する。しかし低濃度の溶液を扱うこと
は、例えばアルコール法でペクチンを回収する場合のよ
うに、莫大な量のアルコールを必要として経済的でな
く、その他の方法によつても製造時の動力費用や生産性
の面から好ましくない。
Under the circumstances, according to the conventional pectin production method, the pectin concentration limit is at most 1%,
If it is higher than this range, the efficiency is lowered due to the difficulty of separating the insoluble residue. However, handling a low-concentration solution is not economical because it requires an enormous amount of alcohol, as in the case of recovering pectin by the alcohol method. It is not preferable in terms of sex.

本発明の目的は、ペクチンの抽出濃度を上げることによ
り、効率よくペクチンを製造する方法を提供することで
あつた。
The object of the present invention was to provide a method for efficiently producing pectin by increasing the extraction concentration of pectin.

本発明は、ペクチン含有植物よりペクチンを抽出して得
られる抽出液又はこの抽出液から分離された不溶解分
に、圧搾助剤を不溶解分100重量部に対し30〜20
0重量部添加し、圧搾して不溶解分を分離したのち、分
離液(圧搾液)を常法により清澄濾過することを特徴と
する、ペクチンの製造方法である。
The present invention relates to an extract obtained by extracting pectin from a pectin-containing plant or an insoluble matter separated from this extract, and a pressing aid in an amount of 30 to 20 per 100 parts by weight of the insoluble matter.
This is a method for producing pectin, which comprises adding 0 parts by weight, pressing to separate insoluble matter, and then clarifying and filtering the separated liquid (pressed liquid) by a conventional method.

本発明によれば、ペクチンの抽出液に圧搾助剤を添加し
混合することにより、不溶解分を硬質化して圧搾を容易
ならしめと共に、圧搾液の流路を確保し、スクリーンの
目詰まりを起こさずに効率よく液を回収することができ
る。
According to the present invention, by adding and mixing the pressing aid to the extract of pectin, the insoluble matter is hardened to facilitate the pressing, and the flow path of the pressing liquid is secured to prevent clogging of the screen. It is possible to efficiently collect the liquid without causing it.

圧搾助剤としては珪藻土、パーライト、セルロース等の
過助剤又はオガ屑、モミ殻、ペクチンの不溶解残査の
水洗物等を使用できるが、不溶解残査を硬質化するとい
う意味ではセルロース、オガ屑、モミ殻等が特に有効で
あり、スクリーンの目詰まり防止の意味からは珪藻土、
パーライト等の過助剤が特に有効である。したがつて
その実際の使用に当つては、その系に適合するようにこ
れらを適宜混合して使用することも有利である。
As the squeezing aid, diatomaceous earth, perlite, a super-helping agent such as cellulose or sawdust, fir shells, washed water of insoluble residue of pectin and the like can be used, but in the sense of hardening the insoluble residue, cellulose, Ogre scraps and fir shells are especially effective, and diatomaceous earth, from the meaning of preventing clogging of the screen,
A super-auxiliary agent such as perlite is particularly effective. Therefore, in the actual use, it is also advantageous to use these by appropriately mixing them so as to be compatible with the system.

圧搾助剤の添加量は、不溶解物の量すなわちペクチンの
濃度に比例して定めることが好ましく、該添加物の種類
やペクチン製造原料にもよるが、絶乾の不溶解分100
重量部に対し一般に30〜200重量部が適当である。
添加量が多すぎる場合には液の回収率が低下して好まし
くないし、逆に少なすぎる場合には十分な圧搾ができな
い。該添加物の添加方法としては、普通は抽出に際して
添加するが、抽出液に添加してもよく、抽出液を遠心分
離等により分離した分離不溶分に該添加物を混合して圧
搾してもよい。圧搾装置としてはネジプレス、ローラー
ミル等の普通の装置が用いられる。
The addition amount of the pressing aid is preferably determined in proportion to the amount of insoluble matter, that is, the concentration of pectin, and although it depends on the type of the additive and the pectin manufacturing raw material, the absolutely dry insoluble matter is 100%.
Generally, 30 to 200 parts by weight is suitable for parts by weight.
If the amount added is too large, the recovery rate of the liquid is lowered, which is not preferable. On the contrary, if it is too small, sufficient pressing cannot be performed. As a method for adding the additive, it is usually added at the time of extraction, but it may be added to the extract, or the additive may be mixed with the separated insoluble matter separated by centrifugation or the like and squeezed. Good. As the squeezing device, a usual device such as a screw press or a roller mill is used.

実施例1 夏みかん搾汁果皮の乾燥物1.5kgを水洗したのち水中に
添加し、全体量を20kgとしたのち塩酸でpHを2.0と
し、90゜Cで30分間攪拌して抽出を行つた。絶乾の不
溶解分は約900gである。次いで抽出液に珪藻土過
助剤70g及びセルロース過助剤400gを混合した
圧搾助剤を用いて圧搾し、不溶解残査3.3kgと搾汁液17.
1kgを得た。搾汁液に珪藻土過助剤を0.5%添加して清
澄過を行い、得られた液に60%濃度となるようイ
ソプロピルアルコールを加え、析出したペクチンの沈殿
を分離し、この沈殿を乾燥、粉砕して粉末ペクチン22
0gを得た。製品ペクチンの原料果皮に対する収率は1
4.7%であり、抽出液のペクチン濃度は1.40%であつ
た。
Example 1 1.5 kg of a dried product of summer orange juice was washed with water, added to water, adjusted to a total amount of 20 kg, adjusted to pH 2.0 with hydrochloric acid, and stirred at 90 ° C. for 30 minutes for extraction. The insoluble matter in the bone dry is about 900 g. Next, the extract was squeezed using a squeezing aid in which 70 g of diatomaceous earth super-assistant and 400 g of cellulose super-assistant were mixed, and 3.3 kg of insoluble residue and juice 17.
I got 1 kg. 0.5% of diatomaceous earth assisting agent was added to the juice and clarification was performed. Isopropyl alcohol was added to the obtained liquid to a concentration of 60% to separate the precipitated pectin precipitate, which was dried and ground. Powder pectin 22
0 g was obtained. Yield of product pectin based on the raw material skin is 1
It was 4.7% and the pectin concentration of the extract was 1.40%.

実施例2 レモンの搾汁果皮の乾燥物1.5kgを実施例1と同様にし
て水洗、抽出し、絶乾の不溶解分850gの抽出液に、
圧搾助剤としてセルロース系過助剤500gを添加
し、圧搾して不溶残査2.6kgと搾汁液17.9kgを得た。以
下実施例1と同様にして清澄過し、脱水、乾燥、粉砕
を行つて粉末ペクチン275gを得た。製品ペクチンの
原料果皮に対する収率は18.3%であり、抽出液のペクチ
ン濃度は1.75%であつた。
Example 2 1.5 kg of the dried product of lemon juice was washed with water and extracted in the same manner as in Example 1 to obtain an extract solution containing 850 g of insoluble matter, which was completely dried.
As a pressing aid, 500 g of a cellulosic super-auxiliary agent was added and pressed to obtain 2.6 kg of an insoluble residue and 17.9 kg of juice. Clarification, dehydration, drying and pulverization were carried out in the same manner as in Example 1 to obtain 275 g of powdered pectin. The yield of the product pectin based on the raw material peel was 18.3%, and the pectin concentration of the extract was 1.75%.

実施例3 夏みかん搾汁果皮の乾燥物2kgを実施例1と同様にして
水洗、抽出し、抽出液に、圧搾助剤としてセルロース
過助剤200g及びモミ殻800gを添加し、圧搾して
不溶解残査3.5kgと搾汁液17.5kgを得た。以下実施例1
と同様にして清澄過し、脱水、乾燥、粉砕を行つて粉
末ペクチン256gを得た。製品ペクチンの原料果皮に
対する収率は12.8%であり、ペクチン濃度は1.83%であ
つた。
Example 3 2 kg of dried dried dried tangerine peel was washed with water and extracted in the same manner as in Example 1, and 200 g of a cellulose super-assisting agent and 800 g of fir shell as a pressing aid were added to the extract and insoluble by pressing. A residue of 3.5 kg and a juice of 17.5 kg were obtained. Example 1 below
Clarification, dehydration, drying and pulverization were carried out in the same manner as in 1. to obtain 256 g of powdered pectin. The yield of the product pectin based on the raw material skin was 12.8%, and the pectin concentration was 1.83%.

比較例1 夏みかん搾汁果皮の乾燥物1kgを実施例1と同様にして
水洗、抽出し、抽出液を圧搾助剤を加えずに遠心分離し
て、残査4.6kgと分離液15.4kgを得た。以下実施例1と
同様して清澄過し、脱水、乾燥、粉砕を行つて粉末ペ
クチン140gを得た。製品ペクチンの原料果皮に対す
る収率は14.0%であり、抽出液の濃度は0.93%であつ
た。この場合は収率は良好であるが、抽出液が低濃度で
ペクチンの製造コストの点で好ましくない。
Comparative Example 1 1 kg of dried dried tangerine peel was washed with water and extracted in the same manner as in Example 1, and the extract was centrifuged without adding a pressing aid to obtain 4.6 kg of a residue and 15.4 kg of a separated liquid. It was Clarification, dehydration, drying and pulverization were carried out in the same manner as in Example 1 to obtain 140 g of powdered pectin. The yield of the product pectin based on the raw material peel was 14.0%, and the concentration of the extract was 0.93%. In this case, the yield is good, but the extract is low in concentration, which is not preferable in terms of pectin production cost.

比較例2 レモンの搾汁果皮の乾燥物1.5kgを実施例1と同様にし
て水洗、抽出し、抽出液を圧搾助剤を加えずに圧搾し
て、不溶解残査1.4kgと搾汁液18.6kgを得た。搾汁液中
に不溶解分が多く、清澄過が困難なため、さらに遠心
分離を行つて残査7.4kgと分離液11.2kgを得た。以下実
施例1と同様にして清澄過し、脱水、乾燥、粉砕を行
つて粉末ペクチン201gを得た。製品ペクチンの原料
果皮に対する収率は13.4%であり、ペクチン濃度は実施
例2のそれと同じである。実施例2と比較して収率が著
しく低下する。
Comparative Example 2 1.5 kg of dried lemon juice peel was washed with water and extracted in the same manner as in Example 1, and the extract was squeezed without adding a squeezing aid to obtain 1.4 kg of insoluble residue and juice of 18.6. I got kg. Since the amount of insoluble matter in the squeezed juice was large and it was difficult to clarify it, further centrifugation was performed to obtain a residue of 7.4 kg and a separated fluid of 11.2 kg. Clarification, dehydration, drying and pulverization were carried out in the same manner as in Example 1 to obtain 201 g of powdered pectin. The yield of the product pectin based on the raw material peel was 13.4%, and the pectin concentration was the same as that of Example 2. The yield is significantly reduced as compared with Example 2.

比較例3 夏みかん搾汁果皮の乾燥物2kgを実施例1と同様にして
水洗、抽出し、絶乾の不溶解分1200gの抽出液にセ
ルロース過助剤200g(不足量)を添加し、圧搾し
て不溶解残査2.1kgと搾汁液18.1kgを得た。搾汁液中に
は不溶解分が多く清澄過が困難なため、さらに遠心分
離を行つて残査8.8kgと分離液9.3kgを得た。以下実施例
1と同様にして清澄過し、脱水、乾燥、粉砕を行つて
粉末ペクチン165gを得た。製品ペクチンの原料果皮
に対する収率は8.3%であり、ペクチン濃度は実施例3
のそれと同じである。実施例3と比較して収率が著しく
低下する。
Comparative Example 3 2 kg of a dried product of summer mandarin orange peel was washed with water and extracted in the same manner as in Example 1, and 200 g (insufficient amount) of a cellulose super-assisting agent was added to an extract solution of 1200 g of absolutely dry insoluble matter, followed by pressing. As a result, 2.1 kg of undissolved residue and 18.1 kg of juice were obtained. Since the squeezed juice contains a large amount of insoluble matter and is difficult to clarify, further centrifugation was performed to obtain a residue of 8.8 kg and a separated solution of 9.3 kg. Clarification, dehydration, drying and pulverization were carried out in the same manner as in Example 1 to obtain 165 g of powdered pectin. The yield of the product pectin based on the raw material peel was 8.3%, and the pectin concentration was determined in Example 3.
It is the same as that of. The yield is significantly reduced as compared with Example 3.

以上の実施例及び比較例から圧搾助剤の添加効果が明ら
かであり、好収率を維持しながらペクチン濃度を高める
ことが可能であることが知られる。
It is known from the above Examples and Comparative Examples that the addition effect of the pressing aid is clear, and it is known that the pectin concentration can be increased while maintaining good yield.

なおこれらの実験で圧搾に用いた装置は、ハンスフエツ
ター社製スクリユープレス、P−スペシヤル型で、スク
リユーの圧縮比1:8のものである。
The device used for squeezing in these experiments is a screen press, P-special type, manufactured by Hans Fetter, and has a screen compression ratio of 1: 8.

───────────────────────────────────────────────────── フロントページの続き (56)参考文献 “大有機化学第20巻天然高分子化合物I I”朝倉書店,昭40−10−30発行,第4 版,P.186−187 “濾過装置”,日刊工業新聞社(昭37. 7.31)P.8及びP.16 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References “Large Organic Chemistry Volume 20 Natural Polymer Compounds II” Asakura Shoten, Sho 40-10-30, 4th edition, p. 186-187 "Filtration device", Nikkan Kogyo Shimbun (sho 37.7.31) P. 8 and P.I. 16

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】ペクチン含有植物よりペクチンを抽出して
得られる抽出液又はこの抽出液から分離された不溶解分
に、圧搾助剤を不溶解分100重量部に対し30〜20
0重量部添加し、圧搾して不溶解分を分離したのち、分
離液を常法により清澄濾過することを特徴とする、ペク
チンの製造方法。
1. A squeezing aid is added to an extract obtained by extracting pectin from a pectin-containing plant or an insoluble matter separated from this extract in an amount of 30 to 20 per 100 parts by weight of the insoluble matter.
A method for producing pectin, which comprises adding 0 part by weight, squeezing to separate insoluble matter, and then clarifying and filtering the separated solution by a conventional method.
JP58238916A 1983-12-20 1983-12-20 Pectin manufacturing method Expired - Lifetime JPH0643445B2 (en)

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JPS60133002A JPS60133002A (en) 1985-07-16
JPH0643445B2 true JPH0643445B2 (en) 1994-06-08

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3511952B2 (en) 1999-01-19 2004-03-29 不二製油株式会社 Pectin, its production method, acidic protein food using the same, and its production method
KR100370962B1 (en) * 2000-07-10 2003-02-06 지성규 Manufacturing meth od of Acetylated pectin for eliminating Endocrine Disrupter from the system

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"大有機化学第20巻天然高分子化合物II"朝倉書店,昭40−10−30発行,第4版,P.186−187
"濾過装置",日刊工業新聞社(昭37.7.31)P.8及びP.16

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