JPH07105A - Purification of non-protein nitrogen component and purified material - Google Patents
Purification of non-protein nitrogen component and purified materialInfo
- Publication number
- JPH07105A JPH07105A JP5168342A JP16834293A JPH07105A JP H07105 A JPH07105 A JP H07105A JP 5168342 A JP5168342 A JP 5168342A JP 16834293 A JP16834293 A JP 16834293A JP H07105 A JPH07105 A JP H07105A
- Authority
- JP
- Japan
- Prior art keywords
- npn
- mother liquor
- desalted
- ion exchange
- protein nitrogen
- 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.)
- Granted
Links
Landscapes
- Dairy Products (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、各種生理活性物質が含
まれる牛乳の非蛋白態窒素成分(以下、NPNというこ
ともある)を精製する方法及びそれによって得られた精
製物に関する。更に詳細には、本発明は、牛乳NPN
を、甘性若しくは酸ホエイを原料として各種膜分離、脱
塩、吸着、酸並びにアルカリ溶出、濃縮、乾燥工程を有
機的に結合して、機能性食品(特定保健用食品)、医薬
品、並びに化粧品原料として利用できる高度に精製され
た精製物を短時間に効率よく製造するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for purifying a non-protein nitrogen component of milk (hereinafter also referred to as NPN) containing various physiologically active substances, and a purified product obtained by the method. More specifically, the present invention relates to milk NPN.
Is organically combined with various types of membrane separation, desalting, adsorption, acid and alkali elution, concentration, and drying steps using sweet or acid whey as a raw material to produce functional foods (foods for specified health uses), pharmaceuticals, and cosmetics. A highly purified product that can be used as a raw material is efficiently produced in a short time.
【0002】[0002]
【従来の技術】一般に、牛乳中には蛋白質以外の非蛋白
態窒素成分が全窒素の5〜6%も含有されていることは
よく知られている。そして、この非蛋白態窒素成分に
は、クレアチニン、尿素、ホスホエタノールアミンなど
の含窒素化合物、グルタミン酸、グリシン、アラニン、
バリン、ロイシンなどのアミノ酸、オロット酸、5′−
CMP、5′−AMP、5′−GMP、5′−UMPな
どの核酸関連物質などきわめて多種類にわたる窒素化合
物が含まれていることも分っている。2. Description of the Related Art Generally, it is well known that milk contains non-protein nitrogen components other than proteins in an amount of 5 to 6% of total nitrogen. And, this non-protein nitrogen component, creatinine, urea, nitrogen-containing compounds such as phosphoethanolamine, glutamic acid, glycine, alanine,
Amino acids such as valine and leucine, orotic acid, 5'-
It is also known that an extremely wide variety of nitrogen compounds such as nucleic acid-related substances such as CMP, 5'-AMP, 5'-GMP, 5'-UMP are contained.
【0003】これ等成分を多量に含む画分を得る方法と
して、原料の限外濾過処理で得られる透過液を濃縮し
て、2段階の結晶分離法により乳糖を除去した母液を脱
塩して粉末化する方法(特開昭60−54637)、並
びに、イオン交換樹脂にこのNPNを吸着させ、脱塩ホ
エイ液でこの樹脂よりNPNを洗い出し、これら成分の
強化されたホエイ濃縮物を製造する方法(特願平3−8
1063)が既に特許出願されており、また、陽、陰両
イオン交換体にNPNを吸着させ、酸及び/又はアルカ
リで溶離回収する方法(特願平4−34062)も特許
出願されている。As a method for obtaining a fraction containing a large amount of these components, the permeated liquid obtained by subjecting the raw material to ultrafiltration is concentrated and the mother liquor from which lactose has been removed is desalted by a two-step crystal separation method. A method of pulverizing (JP-A-60-54637) and a method of adsorbing the NPN on an ion exchange resin and washing the NPN from the resin with a desalting whey solution to produce a whey concentrate fortified with these components. (Japanese Patent Application No. 3-8
No. 1063) has already been applied for a patent, and a method for adsorbing NPN on both positive and anion ion exchangers and eluting and recovering it with an acid and / or an alkali (Japanese Patent Application No. 4-34062) has also been applied for a patent.
【0004】[0004]
【発明が解決しようとする課題】NPNの精製に関して
は、上記のように特許公開ないし特許出願がなされてい
るが、しかしながら、これらの方法によって得られたN
PNには多量の乳糖等不純物を含むため、前記製品は、
NPNを強化した一般食品の原料として利用可能でも、
特定保健用食品、医薬品、化粧品原料としては精製不十
分と判断される。また、これらの方法では、NPNの回
収率が低い、処理時間も長いといった問題点も認められ
る。特に前記製品を化粧品原料にした場合、乳糖を含む
ことから、カビ、酵母が生えやすく、防腐剤の添加が化
粧品によっては必要となる。しかし防腐剤の使用は、防
腐剤をなくすという時代の流れに逆行する結果となる。
また医薬品原料として利用する場合、更に不純物を除去
し、NPN含量を高める必要がある。本発明は濃縮され
たNPNから、灰分や乳糖等不純物を除去し、NPNの
含量を高めて、特定保健用食品はもとより化粧品や医薬
品原料としても応用することを目的とする。Regarding the purification of NPN, the patent publications and patent applications have been made as mentioned above, however, the N obtained by these methods has been proposed.
Since PN contains a large amount of impurities such as lactose,
Even if it can be used as a raw material for general food with enhanced NPN,
It is judged to be insufficiently refined as a raw material for specified health foods, pharmaceuticals, and cosmetics. Further, in these methods, there are problems that the recovery rate of NPN is low and the processing time is long. In particular, when the above product is used as a raw material for cosmetics, since it contains lactose, molds and yeasts tend to grow, and the addition of a preservative is necessary depending on the cosmetic. However, the use of preservatives results in a retrograde trend to the elimination of preservatives.
When used as a drug raw material, it is necessary to further remove impurities and increase the NPN content. It is an object of the present invention to remove impurities such as ash and lactose from concentrated NPN and increase the content of NPN, so that the NPN can be applied not only to foods for specified health uses but also to cosmetics and pharmaceutical raw materials.
【0005】[0005]
【課題を解決するための手段】本発明は、上記目的を達
成するためになされたものであって、各方面から検討し
た結果、NPN原料をそのまま若しくは限外濾過してN
PN母液とし、これを特定のイオン交換膜を装着した電
気透析装置で脱塩した後、イオン交換処理を組み合わせ
ることにより、きわめて効率的にNPNの精製ができる
という新知見を得、この新知見をもとにして更に研究を
重ねた結果、本発明の完成に至ったものである。The present invention has been made in order to achieve the above-mentioned object, and as a result of examinations from various directions, NPN raw material is used as it is or after ultrafiltration.
We obtained a new finding that NPN can be purified very efficiently by combining PN mother liquor, desalting this with an electrodialyzer equipped with a specific ion exchange membrane, and then combining it with ion exchange treatment. As a result of further research, the present invention has been completed.
【0006】先の出願に係る特願平4−34062号に
おいて明らかにされているように、NPN純度を高める
にはイオン交換法が望ましい。しかしながら、NPN回
収率を向上させ、イオン交換処理時間を短縮させるに
は、イオン交換前の母液をNPN阻止率の低い電気透析
膜を用いて脱塩を行うのが効果的である点にはじめて着
目した。また、この時に生じるNPNの一部を含む塩回
収液(濃縮液)とイオン交換体に吸着したNPNの溶離
液を混合、中和した後、この混合液を前の場合とは逆に
NPN阻止率の高い電気透析膜を用いて脱塩することに
より、NPNの高い回収率が得られ、且つNPN純度の
高い精製されたNPN精製物が得られることもはじめて
確認し、更に研究の結果、本発明は完成されたのであ
る。As disclosed in Japanese Patent Application No. 4-34062 related to the previous application, the ion exchange method is desirable for increasing the NPN purity. However, in order to improve the NPN recovery rate and shorten the ion exchange treatment time, it was first noted that it is effective to desalt the mother liquor before ion exchange using an electrodialysis membrane having a low NPN blocking rate. did. In addition, after mixing and neutralizing the salt recovery solution (concentrated solution) containing a part of NPN generated at this time and the eluent of NPN adsorbed on the ion exchanger, the mixed solution is blocked against NPN contrary to the previous case. It was also confirmed for the first time that desalting with an electrodialysis membrane with a high rate yields a high NPN recovery rate and a purified NPN purified product with a high NPN purity can be obtained. The invention has been completed.
【0007】本発明において、精製されるNPN原料と
しては、牛乳、その濃縮物及びその粉末;脱脂乳、その
濃縮物及びその粉末;ホエイ、その濃縮物及びその粉
末;ホエイの限外濾過処理で得られた透過液から乳糖製
造時副産物として得られる母液、その濃縮物及びその粉
末;等NPN含有物がすべて使用可能であり、必要あれ
ば、濃縮物の場合は希釈し、また粉末の場合は溶解する
等の調製処理を行う。In the present invention, as NPN raw materials to be purified, milk, its concentrate and its powder; skim milk, its concentrate and its powder; whey, its concentrate and its powder; The mother liquor obtained as a by-product during the production of lactose from the obtained permeate, its concentrate, and its powder; such NPN-containing materials can all be used, and if necessary, dilute in the case of the concentrate, or in the case of powder, Preparation processing such as dissolution is performed.
【0008】NPN原料はそのまま精製工程に供しても
良いが、イオン交換樹脂等に乳脂肪や高分子の蛋白質が
混入され洗滌に手間取ること等から、NPN原料を限外
濾過(以下、UFということもある)処理して、NPN
を含む透過液(Permeate)と乳脂肪や蛋白質を
含む保留液(Retentate)に分けることが望ま
しい。従ってUF処理を前提に説明する。なお、UF処
理に先立ち、上記したNPN原料類は、UF膜を損傷さ
せぬよう、清浄化してゴミ等を除去することが望まし
い。また、UF膜の分画分子量は、必要とするNPNの
最大分子量によっても相違し格別の限定はないが、1,
000〜50,000程度が好適である。更に、UF装
置に使用される膜としては、格別の限定はなく中空系タ
イプ、ディスクタイプその他が適宜使用可能である。The NPN raw material may be subjected to the purification step as it is, but the NPN raw material is subjected to ultrafiltration (hereinafter referred to as UF) because the milk fat and the high molecular weight protein are mixed in the ion exchange resin and the like and it takes time to wash. There is also) processing, NPN
It is desirable to divide into a permeate containing Permeate and a retentate containing milk fat or protein. Therefore, the UF process will be described as a premise. Prior to the UF treatment, it is desirable that the NPN raw materials described above be cleaned to remove dust and the like so as not to damage the UF film. The molecular weight cutoff of the UF membrane is not particularly limited because it depends on the maximum molecular weight of NPN required.
About 000 to 50,000 is preferable. Further, the membrane used in the UF device is not particularly limited, and a hollow type, a disc type or the like can be appropriately used.
【0009】UF処理で得られた透過液、それを濃縮し
て得た濃縮液、濃縮に際して析出した乳糖を除去した
液、のいずれもが、次に行うNPNの精製工程の原料と
して使用できるので、これらを総称してNPN母液とい
う。Since the permeated liquid obtained by the UF treatment, the concentrated liquid obtained by concentrating the liquid, and the liquid obtained by removing the lactose deposited during the concentration can be used as raw materials for the subsequent NPN purification step. , These are collectively called NPN mother liquor.
【0010】上記のように、UF処理で得られた透過液
は濃度を高めるために濃縮し、これをNPN母液として
使用することが可能なことは上に述べたとおりである。
通常の場合、濃縮度を上げると乳糖が析出するので、こ
れを除去した後の液体もNPN母液として使用可能なこ
とも上で述べたとおりである。透過液の濃縮において、
濃縮は加熱濃縮、真空濃縮、フラッシュ濃縮、逆浸透
(RO)濃縮およびこれ等を組合せた複合濃縮法のいず
れでも良いが、加熱して透過液を長時間高温にさらす
と、乳糖とNPNが反応して、透過液が褐変化するため
に、透過液の加熱温度が低く、且つ短かくしかも能力ア
ップの可能な真空濃縮やフラッシュ濃縮を採用するのが
好ましい。濃縮液から乳糖を析出させ除去するときは、
濃縮液の冷却や結晶缶による方法等、公知の方法を採用
する。また結晶乳糖の大きさは特に規定しないが、NP
Nの収率向上の観点から、種結晶を添加して細かい結晶
をできるだけ多く析出させ、結晶内に不純物を含有させ
ないようにする必要がある。析出した乳糖の除去法は、
遠心分離や濾過等、公知の方法による。これ等3種類の
液体(透過液、濃縮液、乳糖除去液)は、NPN精製工
程の原液となるために以後NPN母液と称することは、
既に述べたとおりである。As described above, the permeate obtained by the UF treatment can be concentrated to increase the concentration and used as the NPN mother liquor.
In the usual case, lactose is precipitated when the concentration is increased, so that the liquid after removing it can also be used as the NPN mother liquor, as described above. In concentrating the permeate,
The concentration may be any of heat concentration, vacuum concentration, flash concentration, reverse osmosis (RO) concentration, and a combined concentration method combining these, but when heated and the permeated liquid is exposed to high temperature for a long time, lactose and NPN react with each other. Then, since the permeated liquid turns brown, it is preferable to employ vacuum concentration or flash concentration, which has a low heating temperature of the permeated liquid and is short and capable of increasing the capacity. When depositing and removing lactose from the concentrate,
A known method such as a method of cooling the concentrated solution or a method using a crystal can is adopted. The size of crystalline lactose is not specified, but NP
From the viewpoint of improving the yield of N, it is necessary to add seed crystals to precipitate as many fine crystals as possible so that impurities are not contained in the crystals. The method of removing the precipitated lactose is
By a known method such as centrifugation or filtration. Since these three types of liquids (permeate, concentrate, lactose remover) are stock solutions for the NPN purification process, they will be referred to as NPN mother liquors hereinafter.
As already mentioned.
【0011】NPN母液には固形分換算で少くとも約5
0%の乳糖、10%の灰分が含まれている。従ってNP
N母液からNPNを精製する方法が種々ある中で、NP
Nをイオン交換体に選択的に吸着させ、これをアルカリ
(若しくは酸)にて溶出、回収する方法が最も効果的で
あり、イオン交換処理法としては特願平4−34062
号に記載されているような既知の方法が適宜使用でき
る。しかし吸着工程でイオン交換体への親和性(選択係
数)は無機イオンよりNPNが劣ると推察されるため、
NPNの吸着量を上げるためには無機イオンを可及的に
除いておくことが望ましい。NPN mother liquor has a solid content of at least about 5
It contains 0% lactose and 10% ash. Therefore NP
Among various methods for purifying NPN from N mother liquor, NP
The most effective method is to selectively adsorb N on an ion exchanger, and elute and recover this with an alkali (or acid). The ion exchange treatment method is disclosed in Japanese Patent Application No. 4-34062.
Known methods such as those described in No. 10 can be appropriately used. However, NPN is inferior to inorganic ion in affinity (selection coefficient) to the ion exchanger in the adsorption step,
In order to increase the adsorption amount of NPN, it is desirable to remove inorganic ions as much as possible.
【0012】脱塩方法としては、(1)イオン交換、
(2)ゲル濾過、(3)ルーズ逆浸透圧処理、(4)電
気透析脱塩といった方法が考えられる。しかしながら、
(1)の方法は、無機塩と同時にNPNもイオン交換体
に吸着するため無機イオンの選択的脱塩可能なイオン交
換体のスクリーニング若しくは開発が必要である。
(2)、(3)の方法は、無機塩とNPNの分子量差が
小さいために溶出位置が近接しており、したがってNP
N母液の脱塩操作が煩雑である。そこで(4)の方法に
ついて種々検討を行った結果、電気透析装置に装着する
イオン交換膜の種類により、最終的に得られる製品での
NPNの回収率が大きく変化するという新しい知見を得
た。本発明はこの現象に着目し、これを効率的に利用し
たものである。以下、本法について説明する。The desalting method includes (1) ion exchange,
Possible methods include (2) gel filtration, (3) loose reverse osmotic pressure treatment, and (4) electrodialysis desalination. However,
The method (1) requires screening or development of an ion exchanger capable of selectively desalting inorganic ions because NPN is adsorbed on the ion exchanger together with the inorganic salt.
In the methods (2) and (3), the elution positions are close to each other because the difference in molecular weight between the inorganic salt and NPN is small, and therefore NP
The desalting operation of N mother liquor is complicated. Therefore, as a result of various studies on the method (4), a new finding was obtained that the NPN recovery rate of the finally obtained product greatly varies depending on the type of the ion exchange membrane attached to the electrodialysis device. The present invention focuses on this phenomenon and utilizes it efficiently. The method will be described below.
【0013】脱塩工程におけるNPNの収率は、イオン
交換膜の種類によって相違するものである。ホエイより
イオン交換体で部分脱蛋白質した液を濃縮した後、乳糖
を結晶分離してなる、部分脱蛋白質−部分脱乳糖ホエイ
(PDPL)を原料とし、NPN阻止率の低いイオン交
換膜として旭硝子社製ED膜(CMV/AMV)を、N
PN阻止率の高いイオン交換膜として旭硝子社製ED膜
(CSV/AMT)をそれぞれ使用した場合の1例を、
下記表1、表2に示した。The yield of NPN in the desalting process varies depending on the type of ion exchange membrane. Asahi Glass Co., Ltd. is used as an ion exchange membrane with a low NPN inhibition rate, which is obtained by concentrating a liquid that has been partially deproteinized from whey with an ion exchanger and then crystallizing lactose. Made ED film (CMV / AMV)
An example of using ED membranes (CSV / AMT) manufactured by Asahi Glass Co., Ltd. as ion exchange membranes with high PN blocking rate
The results are shown in Tables 1 and 2 below.
【0014】[0014]
【表1】 [Table 1]
【0015】[0015]
【表2】 [Table 2]
【0016】PDPLの主要成分組成は、総窒素2.2
%、NPN 1.1%、乳糖48.1%、灰分30.2
%であった。上記した表2の結果から、脱塩したNPN
母液の主要な無機塩はNPN阻止率の高いイオン交換膜
で処理した方が若干高いことがわかり、また表1の結果
から、NPNの収支は約20%も異なることがわかる。The main component composition of PDPL is 2.2 total nitrogen.
%, NPN 1.1%, lactose 48.1%, ash 30.2
%Met. From the results of Table 2 above, desalted NPN
It can be seen that the main inorganic salt of the mother liquor is slightly higher when treated with an ion exchange membrane having a high NPN blocking rate, and the results of Table 1 show that the balance of NPN differs by about 20%.
【0017】このようにして脱塩されたNPN母液(以
下、脱塩NPN母液ということもある)は、イオン交換
体の充填されたカラムに通液し、NPNを本樹脂に吸着
させる。本実験では、イオン交換体は強酸性陽イオン交
換体(三菱化成社:Diaion SK1B)、強塩基
性陰イオン交換体(三菱化成社:Diaion SA1
0A)を用いた。脱塩NPN母液を通液するイオン交換
カラムとしては、イオン交換体を何種類か混合使用する
混床式、一種類の交換体を充填したイオン交換カラムを
使用する単床式、若しくは異なったイオン交換体が充填
されたイオン交換カラムを逐次通液する多床式を採用で
きる。ここでは、これ等を別々に充填して、脱塩NPN
母液を逐次通液する2床式を採用した。The NPN mother liquor desalted in this way (hereinafter, also referred to as desalted NPN mother liquor) is passed through a column packed with an ion exchanger to adsorb NPN onto the resin. In this experiment, the ion exchanger was a strongly acidic cation exchanger (Mitsubishi Kasei: Diaion SK1B), a strongly basic anion exchanger (Mitsubishi Kasei: Diaion SA1).
0A) was used. As the ion exchange column for passing the desalted NPN mother liquor, a mixed bed type using several kinds of ion exchangers, a single bed type using an ion exchange column packed with one kind of exchanger, or different ions A multi-bed type in which an ion exchange column packed with an exchanger is successively passed can be adopted. Here, these are filled separately and desalted NPN
A two-bed system in which the mother liquor is sequentially passed was adopted.
【0018】脱塩NPN母液は、まず強酸性陽イオン交
換体(以下SCI)の充填されたカラムに通液し、つい
で通過液を強塩基性陰イオン交換体(以下SAI)の充
填されたカラムに通液してNPNを吸着させる。NPN
が飽和状態になるまで吸着したSCI、SAIに対し
て、それぞれ2N NaOH、2N H2SO4を通液
し、NPNの脱着、回収を行う。The desalted NPN mother liquor is first passed through a column packed with a strongly acidic cation exchanger (hereinafter referred to as SCI), and then the passing liquid is a column packed with a strongly basic anion exchanger (hereinafter referred to as SAI). To adsorb NPN. NPN
2N NaOH and 2N H 2 SO 4 are passed through the adsorbed SCI and SAI, respectively, until the N is saturated, and NPN is desorbed and collected.
【0019】SCI並びにSAIより、酸並びにアルカ
リ剤にて溶出されたNPN溶出液は、これを混合し、公
知の方法でpH6.0〜7.0に中和する。得られたN
PN溶出液は、NPN母液の脱塩時の塩回収液(濃縮
液)と混合し、NPN阻止率の高いイオン交換膜を装着
した電気透析装置を用いて脱塩し、NPN溶出時並びに
中和時添加した塩類を除去する。脱塩レベルは精製NP
Nの用途に応じて変更する。脱塩後の精製NPNは、再
度濃縮してペースト状若しくは乾燥後粉末化して製品と
する。ここで乾燥は、通気乾燥、噴霧乾燥、凍結乾燥等
公知の乾燥方法を採用し、噴霧乾燥、凍結乾燥以外の乾
燥方法を採用して、ケーキングが起きたときは、粉砕し
て粉末化するとよい。全工程の概略を図1に示す。The NPN eluate eluted from SCI and SAI with an acid and an alkaline agent is mixed and neutralized to pH 6.0 to 7.0 by a known method. Obtained N
The PN eluate is mixed with a salt recovery solution (concentrated solution) at the time of desalting the NPN mother liquor, and desalted using an electrodialysis device equipped with an ion exchange membrane having a high NPN blocking rate, and at the time of NPN elution and neutralization. The salts added at this time are removed. Desalination level is purified NP
Change according to the use of N. The purified NPN after desalting is concentrated again to be a paste or dried and then powdered to obtain a product. Here, for the drying, a known drying method such as aeration drying, spray drying or freeze drying is adopted, and a drying method other than spray drying or freeze drying is adopted, and when caking occurs, it may be pulverized into powder. . The outline of all steps is shown in FIG.
【0020】[0020]
【作用】精製NPNは、脱塩NPN母液をイオン交換体
に吸着させてNPN以外の成分と分離し、これを溶出、
脱塩、回収して得られる。吸着操作に先立ってNPN母
液に含まれるNPNよりイオン交換体に吸着しやすいミ
ネラルを電気透析脱塩により除去する。NPNは
(+),(−)並びに(+)と(−)両方の電荷をもつ
成分が含まれる。従って吸着は陽イオン、陰イオン交換
体の両者を利用し、溶出は、酸又はアルカリを使用す
る。In the purified NPN, the demineralized NPN mother liquor is adsorbed on the ion exchanger to separate it from the components other than NPN, and this is eluted.
Obtained by desalting and collecting. Prior to the adsorption operation, minerals that are more easily adsorbed on the ion exchanger than NPN contained in the NPN mother liquor are removed by electrodialysis desalting. NPN includes (+), (-) and components having both (+) and (-) charges. Therefore, adsorption uses both cations and anion exchangers, and elution uses acid or alkali.
【0021】以下に本発明の実施例について述べる。Examples of the present invention will be described below.
【0022】[0022]
【実施例1】PDPL 10%溶液を分画分子量20,
000のUF処理し、得られたNPN母液を旭硝子社製
ED膜(CMV/AMV)で電気伝導度を指標として9
7%電気透析脱塩し、脱塩NPN母液及び塩回収液とし
た。この脱塩NPN母液を、SCIを充填したカラムに
SV=3で通液し、イオン交換体体積の45倍相当量
(45BV)を通液した後、5BVの水でカラム内のS
CIを水洗した。SCIは三菱化成社製Diaion
SK1Bを使用した。SCIに未吸着のNPNは全NP
Nの49%であった。水洗後、2BVの2NのNaOH
を循環し、延6BV通液してNPNを溶出した。後、5
BVの水でカラム並びにSCIを水洗し、残液を回収し
た。アルカリ溶出(水洗水含む)で通液した全NPNの
18%を回収した。Example 1 A 10% solution of PDPL was used to cut off a molecular weight of 20,
000 UF treatment, and the NPN mother liquor obtained was ED film (CMV / AMV) manufactured by Asahi Glass Co., Ltd.
It was desalted by 7% electrodialysis to obtain a desalted NPN mother liquor and a salt recovery liquid. This desalted NPN mother liquor was passed through a column filled with SCI at SV = 3, a volume equivalent to 45 times the ion exchanger volume (45 BV) was passed, and then 5 BV of water was added to the S in the column.
The CI was washed with water. SCI is Mitsubishi Kasei's Diaion
SK1B was used. NPN not adsorbed on SCI is all NP
It was 49% of N. After washing with water, 2BV of 2N NaOH
NPN was eluted by circulating 6BV. After 5
The column and SCI were washed with BV water to collect the residual liquid. 18% of all NPN passed through by elution with alkali (including washing water) was recovered.
【0023】SCIを通過した脱塩NPN母液並びに母
液の水洗水はSCIの1.1倍のSAIを充填したカラ
ムにSV=3で通液し、44BV通液した後5BVの水
でカラム内のSAIを水洗した。SAIは三菱化成社製
Diaion SA10Aを使用した。SAIに未吸着
のNPNは全NPNの11%であった。The desalted NPN mother liquor passing through the SCI and the washing water of the mother liquor were passed through a column packed with SAI at 1.1 times the SCI at SV = 3, and after passing 44 BV, 5 BV of water in the column. The SAI was washed with water. As SAI, Mitsubishi Kasei's Diaion SA10A was used. NPN not adsorbed on SAI was 11% of all NPN.
【0024】水洗したSAIに2BVの2NのH2SO4
を循環し、延8BV通液してNPNを溶出した。後、5
BVの水でカラム並びにSCIを水洗し、残液を回収し
た。本工程の酸溶出(水洗水含む)でNPNの17%を
回収した。物質収支は下記表3、表4の通りであった。2BV of 2N H 2 SO 4 was added to the washed SAI.
NPN was eluted by circulating 8BV of the solution. After 5
The column and SCI were washed with BV water to collect the residual liquid. 17% of NPN was recovered by acid elution (including washing water) in this step. The material balance is shown in Tables 3 and 4 below.
【0025】[0025]
【表3】 [Table 3]
【0026】[0026]
【表4】 [Table 4]
【0027】上記結果から明らかなように、全イオン交
換体から回収されたNPNは、脱塩NPN母液の68%
であった。これ等SKlB吸着画分溶離液、SA10A
吸着画分溶離液及びED濃縮液(塩回収液)からなるN
PN溶出液を混合し、中和後、旭硝子社製ED膜(CS
V/AMT)で電気透析脱塩したところ、固形分当り、
74%のNPN(N×6.38)を含むNPN溶液が得
られ、NPNの収率は約30%であった。As is clear from the above results, NPN recovered from all ion exchangers was 68% of the desalted NPN mother liquor.
Met. These SKIB adsorption fraction eluent, SA10A
N consisting of adsorption fraction eluent and ED concentrate (salt recovery solution)
After mixing and neutralizing the PN eluate, Asahi Glass ED membrane (CS
Electrodialysis desalination with V / AMT)
An NPN solution containing 74% NPN (N × 6.38) was obtained, and the NPN yield was about 30%.
【0028】また、イオン交換樹脂処理前の電気透析処
理を、本法とは逆にNPN阻止率の高いイオン交換膜
(旭硝子社製ED膜(CSV/AMT))を用いて行っ
た場合のNPNの物質収支も併せて表3に示したが、最
終的に得られるNPN画分のNPN回収率は本法の約1
/2にすぎなかった。NPN in the case where the electrodialysis treatment before the ion exchange resin treatment is carried out using an ion exchange membrane (ED membrane (CSV / AMT) manufactured by Asahi Glass Co., Ltd.) having a high NPN blocking rate contrary to the present method. Table 3 also shows the mass balance of NPN. The NPN recovery rate of the finally obtained NPN fraction is about 1 of this method.
It was only / 2.
【0029】[0029]
【発明の効果】牛乳に含まれるNPNの中には種々の生
理活性物質が多量に含まれる。しかし、従来のNPN精
製物には乳糖等多くの不純物を含むため、医薬品や化粧
品原料としての活用は不可能であった。本発明によりこ
うした不純物を除去して、精製することにより、特定保
健用食品、医薬品、化粧品原料として利用することがで
きる。また、本発明は、処理時間を短縮し、しかもNP
N回収率は大幅に向上せしめることのできる新規な工業
的なNPN精製法も提供するものである。The NPN contained in milk contains a large amount of various physiologically active substances. However, conventional NPN purified products contain many impurities such as lactose, and thus cannot be used as raw materials for medicines and cosmetics. By removing such impurities and purifying according to the present invention, they can be used as raw materials for specified health foods, pharmaceuticals and cosmetics. Further, the present invention shortens the processing time, and further, the NP
It also provides a novel industrial NPN purification method that can significantly improve the N recovery rate.
【図1】NPN精製工程概略図である。FIG. 1 is a schematic diagram of an NPN purification process.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 大津 俊広 東京都東村山市栄町1−21−3 明治乳業 株式会社中央研究所内 (72)発明者 桑田 有 東京都東村山市栄町1−21−3 明治乳業 株式会社中央研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Toshihiro Otsu 1-21-3 Sakaemachi, Higashimurayama, Tokyo Meiji Dairy Industry Co., Ltd. (72) Inventor Yu Kuwata 1-2-1-3 Sakaemachi, Higashimurayama, Tokyo Meiji Dairy Central Research Institute Co., Ltd.
Claims (8)
電気透析脱塩処理して回収した塩回収画分(NPNの一
部を含有する濃縮液)、及び/又は、上記により脱塩さ
れた脱塩NPN母液をイオン交換樹脂処理し溶離回収さ
れたNPN画分を、NPN阻止率の高いイオン交換膜を
装着した電気透析装置を用いて脱塩処理し、NPNを精
製することを特徴とする非蛋白態窒素成分の精製法。1. A salt recovery fraction (concentrated solution containing a part of NPN) recovered by electrodialysis desalting a non-protein nitrogen component (NPN) -containing raw material, and / or desalted as described above. The demineralized NPN mother liquor is treated with an ion exchange resin, and the NPN fraction eluted and collected is desalted using an electrodialysis device equipped with an ion exchange membrane having a high NPN blocking rate to purify NPN. A method for purifying non-protein nitrogen components.
限外濾過透過液を、NPN阻止率の低いイオン交換膜を
装置した電気透析装置を用いて脱塩処理した後に脱塩N
PN母液とし、次いで脱塩NPN母液をイオン交換樹脂
処理して、NPNを樹脂に吸着せしめ水洗した後にNP
Nを樹脂より脱着せしめることを特徴とする非蛋白態窒
素成分の精製法。2. The NPN-containing raw material as it is or the ultrafiltration permeate thereof is subjected to a desalting treatment using an electrodialysis device equipped with an ion exchange membrane having a low NPN rejection ratio, and then desalted N.
PN mother liquor, then deionized NPN mother liquor is treated with ion exchange resin, NPN is adsorbed on the resin and washed with water, then NP
A method for purifying non-protein nitrogen components, characterized in that N is desorbed from the resin.
得られる透過液、該透過液の濃縮液、及び/又は該透過
液から乳糖を分離した後の液体を使用することを特徴と
する請求項2に記載の精製法。3. A permeated liquid obtained by an ultrafiltration treatment, a concentrated liquid of the permeated liquid, and / or a liquid obtained by separating lactose from the permeated liquid is used as the ultrafiltration permeated liquid. The purification method according to claim 2.
電気透析膜を装着した電気透析装置を用いて脱塩し、脱
塩されたNPN母液は、これをイオン交換樹脂処理して
NPN画分を吸着回収し、上記脱塩処理によって回収さ
れた塩回収画分(NPNの一部を含有する濃縮液)と合
し、得られた混合物を中和した後、NPN阻止率の高い
電気透析膜を装着した電気透析装置を用いて脱塩処理
し、NPNを精製することを特徴とする非蛋白態窒素成
分の精製法。4. The NPN-containing raw material is desalted by using an electrodialysis device equipped with an electrodialysis membrane having a low NPN blocking rate, and the desalted NPN mother liquor is treated with an ion exchange resin to obtain an NPN fraction. Is adsorbed and collected, and is combined with the salt-recovered fraction (concentrated solution containing a part of NPN) collected by the desalting treatment, and the resulting mixture is neutralized, and then an electrodialysis membrane having a high NPN blocking rate is obtained. A method for purifying a non-protein nitrogen component, which comprises purifying NPN by desalting using an electrodialysis device equipped with.
換樹脂処理及び陰イオン交換樹脂処理を組み合わせて行
うことを特徴とする請求項1〜請求項4のいずれか1項
に記載の精製法。5. The purification method according to claim 1, wherein the ion exchange resin treatment is performed by combining a cation exchange resin treatment and an anion exchange resin treatment.
びその粉末;脱脂乳、その濃縮物及びその粉末;ホエ
イ、その濃縮物及びその粉末;ホエイの限外濾過処理で
得られた透過液から乳糖製造時副産物として得られる母
液、その濃縮物及びその粉末;からなる群から選ばれる
ものであり、必要あれば、濃縮物の場合は希釈し、また
粉末の場合は溶解することを特徴とする請求項1〜請求
項5のいずれか1項に記載の精製法。6. An NPN-containing raw material is milk, its concentrate and its powder; skim milk, its concentrate and its powder; whey, its concentrate and its powder; permeate obtained by ultrafiltration treatment of whey. A mother liquor obtained as a by-product during the production of lactose from the above, a concentrate thereof and a powder thereof; and, if necessary, the concentrate is diluted and the powder is dissolved. The purification method according to any one of claims 1 to 5.
載の精製法によって得られた、NPN含量が高く乳糖含
量は低い精製された非蛋白態窒素成分。7. A purified non-protein nitrogen component having a high NPN content and a low lactose content, which is obtained by the purification method according to any one of claims 1 to 6.
脱塩処理した後、濃縮及び/又は粉末化してなる精製さ
れた非蛋白態窒素成分。8. The purified NPN according to claim 7,
A purified non-protein nitrogen component obtained by desalting and then concentrating and / or pulverizing.
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