JPH03223299A - Production of disodium 5'-guanylate. disodium 5'-inosinate mixed crystal - Google Patents
Production of disodium 5'-guanylate. disodium 5'-inosinate mixed crystalInfo
- Publication number
- JPH03223299A JPH03223299A JP2016663A JP1666390A JPH03223299A JP H03223299 A JPH03223299 A JP H03223299A JP 2016663 A JP2016663 A JP 2016663A JP 1666390 A JP1666390 A JP 1666390A JP H03223299 A JPH03223299 A JP H03223299A
- Authority
- JP
- Japan
- Prior art keywords
- disodium
- crystal
- mixed crystal
- inosinate
- crystals
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 113
- AANLCWYVVNBGEE-IDIVVRGQSA-L Disodium inosinate Chemical compound [Na+].[Na+].O[C@@H]1[C@H](O)[C@@H](COP([O-])([O-])=O)O[C@H]1N1C(NC=NC2=O)=C2N=C1 AANLCWYVVNBGEE-IDIVVRGQSA-L 0.000 title claims abstract description 13
- 235000013890 disodium inosinate Nutrition 0.000 title claims abstract description 13
- PVBRXXAAPNGWGE-LGVAUZIVSA-L disodium 5'-guanylate Chemical compound [Na+].[Na+].C1=2NC(N)=NC(=O)C=2N=CN1[C@@H]1O[C@H](COP([O-])([O-])=O)[C@@H](O)[C@H]1O PVBRXXAAPNGWGE-LGVAUZIVSA-L 0.000 title claims abstract description 6
- 235000013896 disodium guanylate Nutrition 0.000 title claims abstract description 6
- 239000004193 disodium 5'-ribonucleotide Substances 0.000 title claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 239000004194 disodium inosinate Substances 0.000 claims abstract description 13
- 239000004198 disodium guanylate Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 7
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 23
- 238000002425 crystallisation Methods 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- 230000008025 crystallization Effects 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000012452 mother liquor Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004278 EU approved seasoning Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011549 crystallization solution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002773 nucleotide Substances 0.000 description 1
- 125000003729 nucleotide group Chemical group 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野１
本発明は、調味料、医薬品等として有用な５゛ヌクレオ
チド混物、特に５“ −グアニル酸ジナトリウムと５゛
−イノシン酸ジナトリウムの混合物をその混晶として
製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field 1] The present invention is directed to a mixture of 5' nucleotides useful as seasonings, pharmaceuticals, etc., particularly a mixture of disodium 5'-guanylate and disodium 5'-inosinate. The present invention relates to a method for producing a mixed crystal thereof.
［従来の技術〕
５゛−イノシン酸ジナトリウム（以下、ＩＮと略す）と
５°−グアニル酸ジナトリウム（以下、ＧＮと略す）を
混晶の形態で製造する方法として次の二つの方法及び本
発明者らが見い出した方法がある。[Prior Art] The following two methods are available for producing 5'-disodium inosinate (hereinafter abbreviated as IN) and 5'-disodium guanylate (hereinafter abbreviated as GN) in the form of mixed crystals. There is a method discovered by the present inventors.
＋１１ ＩＮとＧＮを、メタノール等の有機溶媒含有
溶液にＩＮとＧＮを溶解し、これからＩＮとＧＮの混晶
（以下、ＩＮ −ＧＮ混晶と略す）を得る方法（特公昭
４〇−１２９１４号公報）。+11 A method for obtaining a mixed crystal of IN and GN (hereinafter abbreviated as IN-GN mixed crystal) by dissolving IN and GN in a solution containing an organic solvent such as methanol (Japanese Patent Publication No. 40-12914) Public bulletin).
（２１ＩＮとＧＮを水に溶解し、冷却または濃縮晶析に
よりＩＮ／ＧＮ混晶を得る方法（特公昭５４−１６５８
２号、同５５−４７８７７号公報）。(21Method of dissolving IN and GN in water and obtaining IN/GN mixed crystal by cooling or concentrating crystallization (Japanese Patent Publication No. 54-1658
No. 2, Publication No. 55-47877).
１３１ ＧＮが液底体として存在するＧＮ含有スラリ
ー溶液に、ＩＮ含有水溶液を徐々に添加してＩＮ −Ｇ
Ｎの混晶を生成させることを特徴とする方法（特願平１
−２２８８９９号公報）。131 IN-G is obtained by gradually adding an IN-containing aqueous solution to a GN-containing slurry solution in which GN exists as a liquid bottom body.
A method characterized by producing a mixed crystal of N (Patent Application No. 1999)
-228899).
ｒＮとＧＮは、メタノール等の有機溶媒含有水溶液また
は水溶液中で、ＩＮの結晶格子にＧＮを取り込む形で混
晶を形成することが知られている。この混晶のＸ線回折
図はほぼＩＮのＸ線回折図と同じパターンを示し、化学
構造の類領したＧＮがＩＮの格子に入り、水素結合によ
り安定状態を保つものと考えられている。 ＩＮの結晶
は結晶生長性がよく、このＩＮ結晶の格子中にＧＮが取
り込まれた混晶の特性も、ＩＮの結晶とほぼ同等のもの
となる。It is known that rN and GN form a mixed crystal by incorporating GN into the crystal lattice of IN in an aqueous solution or an aqueous solution containing an organic solvent such as methanol. The X-ray diffraction diagram of this mixed crystal shows almost the same pattern as the X-ray diffraction diagram of IN, and it is thought that GN, which has a similar chemical structure, enters the lattice of IN and maintains a stable state through hydrogen bonding. The IN crystal has good crystal growth, and the characteristics of the mixed crystal in which GN is incorporated into the lattice of the IN crystal are almost the same as those of the IN crystal.
ＩＮ・ＧＮ混晶を取得する際に、前記（１）の方法では
高い回収率で晶析できるものの、工業的にはメタノール
等の有機溶媒を使用するために防爆など高価な設備を要
し、製造コストも高くなる欠点がある。また、（２）の
方法では、製品の規格として十分な精度の晶析を行うた
めには、濃縮ドレン、フィード液の管理や温度、圧力等
の設定条件を厳しく制御する必要があり、装置の複雑化
と共に、設備費も膨大なものとなる。さらに、βの方法
では晶析母液を用いて目的の組成の混晶を得ることは困
難である。When obtaining IN/GN mixed crystals, although the method (1) above can crystallize with a high recovery rate, industrially it requires expensive equipment such as explosion-proof equipment due to the use of organic solvents such as methanol. The disadvantage is that the manufacturing cost is also high. In addition, in method (2), in order to perform crystallization with sufficient precision to meet product standards, it is necessary to strictly control the management of concentrated drain and feed liquid, and the setting conditions such as temperature and pressure. As the complexity increases, equipment costs also increase. Furthermore, in the method β, it is difficult to obtain a mixed crystal with a desired composition using a crystallization mother liquor.
次に（３）の方法は上記（１１、（２）の問題点が解決
され、水晶析法により、ＩＮ −ＧＮ混晶を製造する際
に、ＩＮとＧＮの比率を自由にコントロールすることが
でき、しかもその晶析母液は、その組成を厳密にコント
ロールせずにリサイクルさせてＧＮを添加したＧＮ含有
スラリー溶液をつくるだけで母液から連続して混晶を取
得することができる。さらに設備も簡単で安価に製造で
きるなど、画期的な特徴を持っている。しかしながら、
この晶析法により得られる結晶は、鱗片状で平均粒径が
小さい、流動性が悪い、等の好ましくない粉体特性を存
している。この為、固液分離操作に手間取る等の問題が
あった。Next, method (3) solves the problems of (11 and (2) above) and allows the ratio of IN and GN to be freely controlled when producing an IN-GN mixed crystal using the crystallization method. Moreover, mixed crystals can be obtained continuously from the mother liquor by simply recycling the crystallization mother liquor without strictly controlling its composition and creating a GN-containing slurry solution with GN added. It has revolutionary features such as being easy and inexpensive to manufacture.However,
The crystals obtained by this crystallization method have unfavorable powder characteristics such as scale-like shape, small average particle size, and poor fluidity. For this reason, there were problems such as a time-consuming solid-liquid separation operation.
［発明が解決しようとする課題］
本発明の問題は、ＩＮ −ＧＮ混晶の晶析法に関し、好
ましい粉体特性を有するＩＮ −ＧＮ混晶を製造するこ
とにある。[Problems to be Solved by the Invention] The problem of the present invention is to produce an IN-GN mixed crystal having preferable powder properties, regarding a method for crystallizing an IN-GN mixed crystal.
［課題を解決するための手段］
本発明者らはＩＮ −ＧＮ混晶の粉体特性を改良するべ
く鋭意検討を重ねた結果、「従来の技術」中の（３）の
方法で晶析を行う際に、種晶としてＩＮ結晶、またはＩ
Ｎ −ＧＮ混晶を添加することにより、厚みのある板状
結晶で、平均粒径が大きい、流動性が優れている等の好
ましい粉体特性を有する結晶を見い出し、本発明を完成
するに至った。[Means for Solving the Problems] As a result of intensive studies to improve the powder properties of IN-GN mixed crystals, the present inventors conducted crystallization using the method (3) in the "prior art". When carrying out, IN crystal or I crystal is used as a seed crystal.
By adding N-GN mixed crystals, we discovered thick plate-shaped crystals with favorable powder characteristics such as large average particle size and excellent fluidity, and completed the present invention. Ta.
すなわち、本発明は、５° −グアニル酸ジナトリウム
含有スラリー溶液に５′ −イノシン酸ジナトリウム含
有溶解液を添加して混晶を生成せしめるに際し、５゛
−イノシン酸ジナトリウムを添加する前若しくは添加し
た後に種晶として５” −イノシン酸ジナトリウム結晶
または５゛グアニル酸ジナトリウム・イノシン酸ジナト
リウム混晶を添加せしめることを特徴とする５° −グ
アニル酸ジナトリウム・５゛ −イノシン酸ジナトリウ
ム混晶の製造方法に関する。That is, in the present invention, when adding a solution containing 5'-disodium inosinate to a slurry solution containing 5'-disodium guanylate to generate a mixed crystal,
-5°-guanyl characterized by adding 5"-disodium inosinate crystals or 5" disodium guanylate/disodium inosinate mixed crystals as seed crystals before or after adding disodium inosinate. The present invention relates to a method for producing disodium acid/disodium 5'-inosinate mixed crystal.
本発明に用いる種晶は発酵法、有機合成法などにより取
得されるＩＮ結晶またはＩＮ −ＧＮ混晶が使用できる
。さらに好ましい種晶は、その形状が球状または厚みの
ある結晶である。鱗片状の結晶を種晶として用いること
は好ましくない。なぜなら、種晶を成長せしめて得られ
る結晶も鱗片状になってしまうためで、これは、鱗片状
の種晶の結晶成長点が制限されているため、一方向のみ
の結晶成長が促進されると考えられる。種晶の平均粒径
は、３０μｍ〜１５０μｍ、好ましくは５０μｍ〜１０
０μｍが良い。種晶の量は、ＧＮ含有スラリー溶液のＧ
Ｎ重量に対し、ＩＮで２〜２０％、ＩＮ −ＧＮ混晶で
５〜３０％、好ましくはＩＮで５〜ｌＯ％、ＩＮ・ＧＮ
混晶で５〜１５％が良い。As the seed crystals used in the present invention, IN crystals or IN-GN mixed crystals obtained by fermentation methods, organic synthesis methods, etc. can be used. More preferred seed crystals are spherical or thick crystals. It is not preferable to use scaly crystals as seed crystals. This is because the crystals obtained by growing seed crystals also become scaly. This is because the crystal growth points of scaly seed crystals are restricted, which promotes crystal growth in only one direction. it is conceivable that. The average particle size of the seed crystals is 30 μm to 150 μm, preferably 50 μm to 10 μm.
0 μm is good. The amount of seed crystals is determined by the amount of G in the GN-containing slurry solution.
Based on the weight of N, 2 to 20% of IN, 5 to 30% of IN-GN mixed crystal, preferably 5 to 10% of IN, IN/GN
A mixed crystal content of 5 to 15% is good.
次に、本発明で用いるＧＮ含有スラリー溶液は主にＧＮ
を水に懸濁したものが使用される。このＧＮ含有スラリ
ー溶液は若干量の有機溶媒を含んでいてもよいが、好ま
しくは水のみの系である。ここで、当初に用いるＧＮの
結晶形態は、α晶、β晶、Ｔ晶のいずれでも良く、限定
されない。さらにＧＮＮ含有スラリー液液ＩＮ、原料由
来の不純物無機塩類等を含んでも良いが、それらの含有
は、目的の混晶を生成させる過程で、種晶以外のＩＮ結
晶が析出しない濃度に限定される。このＧＮ含有スラリ
ー溶液を一定の温度に保ちつつ、ＩＮ含有溶解液、好ま
しくはその飽和溶液を徐々に加えて、ＧＮの液底体が完
全にＩＮとの混晶に変化したところを顕微鏡等で結晶状
態を確認し、晶析終了とする。種晶の添加時期は、ＧＮ
含有スラリー溶液にＩＮ含有溶解液を添加する前であっ
ても後であってもよい。なお、ＩＮ含有溶解液には、Ｇ
Ｎ、原料由来の不純物無機塩類等を含んでも良いが、Ｉ
Ｎ −ＧＮ混晶を生成できる条件に限定される。晶析の
際、ＩＮ含有溶解液は混晶の晶析率を向上させるため、
高温で飽和濃度に近いものを使用するのがよい。もちろ
ん、ＩＮ含有溶解液が高温である場合には、晶析液の温
度が急上昇しないように注意する必要がある。ＩＮ含有
溶解液の添加はできるだけゆっくり行うのがよい。これ
は、ＩＮ含有溶解液が急冷されて、ＩＮとして晶析し、
器壁に付着したり、晶析槽内に沈降してＩＮ過剰の混晶
が生成する事などを回避するためである。Next, the GN-containing slurry solution used in the present invention mainly consists of GN.
is used suspended in water. This GN-containing slurry solution may contain a small amount of organic solvent, but is preferably a water-only system. Here, the crystal form of GN used initially may be any of α crystal, β crystal, and T crystal, and is not limited. Furthermore, GNN-containing slurry liquid IN, impurity inorganic salts derived from raw materials, etc. may be included, but their inclusion is limited to a concentration that will not precipitate IN crystals other than seed crystals during the process of generating the desired mixed crystal. . While maintaining this GN-containing slurry solution at a constant temperature, gradually add an IN-containing solution, preferably a saturated solution thereof, and observe with a microscope etc. when the liquid base of GN has completely changed into a mixed crystal with IN. Confirm the crystal state and conclude crystallization. The timing of adding seed crystals is GN
This may be done before or after adding the IN-containing solution to the slurry solution. Note that the IN-containing solution contains G
N, impurities derived from raw materials, inorganic salts, etc. may be included, but I
The conditions are limited to those that can produce N-GN mixed crystal. During crystallization, the IN-containing solution improves the crystallization rate of mixed crystals, so
It is best to use something close to saturation concentration at high temperature. Of course, when the IN-containing solution is at a high temperature, care must be taken to prevent the temperature of the crystallization solution from rising rapidly. It is preferable to add the IN-containing solution as slowly as possible. This is because the IN-containing solution is rapidly cooled and crystallized as IN.
This is to avoid the formation of mixed crystals containing excess IN by adhering to the vessel wall or settling in the crystallization tank.
また、晶析率向上のために、これらの水溶液に、ＮａＣ
ｌ 、 ＮａｚＳＯａ、ＮＨ，ＳＯ，、ＮＨ４ＣＡ’
、 （ＮＨｉ）ｚｓＯ４などの塩を加えて塩析をかけ、
溶解度の小さいところで晶析を行うことも有効である。In addition, in order to improve the crystallization rate, NaC was added to these aqueous solutions.
l, NazSOa, NH,SO,, NH4CA'
, add salt such as (NHi)zsO4 and salt out,
It is also effective to perform crystallization at a location with low solubility.
混晶のＩＮとＧＮの組成を変えるためには、晶析温度を
例えば２０℃、３０℃、４０℃、５０℃等と変えれば良
く、その温度の共通溶解度に対応する晶析が行われ、混
晶中の組成を自由に設定することが出来る。In order to change the composition of IN and GN in the mixed crystal, it is sufficient to change the crystallization temperature to, for example, 20°C, 30°C, 40°C, 50°C, etc., and crystallization corresponding to the common solubility at that temperature is performed. The composition in the mixed crystal can be set freely.
晶析操作を例えば３０℃以上の温度で行えばＧＮのα晶
が混晶に変化する。一方、２０℃等の低温で行うと、Ｇ
Ｎはβ晶で存在するが、この場合においてもβ晶が混晶
に変化する事が確認されており、晶析操作は同じでよい
。If the crystallization operation is performed at a temperature of 30° C. or higher, for example, the α crystal of GN changes to a mixed crystal. On the other hand, when carried out at a low temperature such as 20℃, G
Although N exists in the form of a β crystal, it has been confirmed that the β crystal changes to a mixed crystal even in this case, and the crystallization operation may be the same.
また晶析するＧＮ含有スラリー溶液、ＩＮ含有水溶液の
ｐ）Ｉについては、これらがジナトリウム塩の領域、す
なわち、ＧＮについてはｐＨ６〜１０、ＩＮについては
ｐＨ６〜１０の範囲にあれば、特に制限されることなく
混晶を得ることが出来る。Furthermore, p)I of the GN-containing slurry solution and IN-containing aqueous solution to be crystallized is particularly limited if they are in the disodium salt range, that is, in the range of pH 6 to 10 for GN and pH 6 to 10 for IN. It is possible to obtain a mixed crystal without being damaged.
ＧＮ（β晶）８４０ｇを塩化ナトリウム２４０ｇをふく
む２４００ ｇの水に分解させてＧＮ （α晶）含有ス
ラリー溶液とし、このスラリーの温度を４０℃とした。840 g of GN (β crystal) was decomposed into 2400 g of water containing 240 g of sodium chloride to obtain a slurry solution containing GN (α crystal), and the temperature of this slurry was set to 40°C.
６Ｎはこの塩濃度、温度ではα晶に転移した。これに、
すり鉢ですりつぶし、粒径を７０μ−〜１２０μｍに整
えたＩＮ −ＧＮ混晶を種晶として２５０ｇ加え、その
後、ｌＮ６４０ｇを７０℃で加熱溶解した３５２０ ｇ
の塩化ナトリウム水溶液（ＮａＣ１３２０ｇ）をかくは
んしながら徐々に添加した。At this salt concentration and temperature, 6N transformed into an α crystal. to this,
Add 250 g of IN-GN mixed crystal as a seed crystal, which was ground in a mortar and adjusted to a particle size of 70 μm to 120 μm, and then 3520 g of 640 g of IN-GN was dissolved by heating at 70°C.
An aqueous sodium chloride solution (1320 g of NaC) was gradually added with stirring.
ＧＮα晶は徐々に混晶に変化して行き、ＧＮα晶が完全
に消失したときを顕微鏡で確認し、終点とした。顕微鏡
で観察すると、種晶が徐々に成長して大きな結晶になっ
て行くのが認められた。晶析していたＩＮ−ＧＮ混晶を
卓上振り切りで分離し、風乾した。混晶の収量は８００
ｇであった。The GNα crystals gradually changed into mixed crystals, and the end point was confirmed using a microscope when the GNα crystals completely disappeared. When observed under a microscope, it was observed that the seed crystals gradually grew into large crystals. The IN-GN mixed crystal that had been crystallized was separated using a tabletop shaker and air-dried. The yield of mixed crystals is 800
It was g.
なお、結晶分離時の母液の分離性はきわめて良好であっ
た。Note that the separation of the mother liquor during crystal separation was extremely good.
次に、ここで得られた混晶と種晶を添加しない場合で得
られる混晶と粉体特性について比較して示した。すなわ
ち同濃度のＧＮ、 ＩＮ溶液を種晶を入れずに４０°Ｃ
で晶析したもの（従来法（特願平１２２８８９９号公報
記載の方法）による混晶）と比較した。結果は下表の通
りである。Next, the powder properties of the mixed crystal obtained here and the mixed crystal obtained without adding seed crystals were compared. That is, GN and IN solutions of the same concentration were heated at 40°C without seed crystals.
(mixed crystal obtained by the conventional method (method described in Japanese Patent Application No. 1228899)). The results are shown in the table below.
＊流動性指数： Ｃａｒｒ法による
＊圧縮率：Ｃ＝１００※（Ｐ−Ａ）／ＰＰ；かさ密比重
Ａ；かさ粗比重
＊平均粒径：レーザー散乱法による
＊流動性測定：細用ミクロン■製パウダーテスターによ
る
以上の結果から、本発明方法により得られる混晶の粉体
特性は、従来法で得られるものより優れていた
実施例２
ＧＮｒ晶２３．５Ｋｇを塩化ナトリウム４．７Ｋｇを含
む４８．８Ｋｇの水に分散させてＧＮα晶を析出させ、
このスラリーの温度を３５℃とした。種晶としてＩＮ結
晶２．５７ＫｇをＧＮ含有スラリー溶液に添加した後、
ＩＮ結晶１４．５Ｋｇを塩化ナトリウム５．３Ｋｇを含
む５３．８Ｋｇの水（７０℃）に溶解させたものを徐々
に添加した。*Fluidity index: According to Carr method *Compressibility: C=100*(P-A)/PP; Bulk density specific gravity A; Bulk coarse specific gravity *Average particle size: According to laser scattering method *Fluidity measurement: Fine micron■ From the above results obtained using the manufactured powder tester, the powder properties of the mixed crystal obtained by the method of the present invention were superior to those obtained by the conventional method. .Disperse in 8 kg of water to precipitate GNα crystals,
The temperature of this slurry was 35°C. After adding 2.57 kg of IN crystals as seed crystals to the GN-containing slurry solution,
A solution of 14.5 kg of IN crystals dissolved in 53.8 kg of water (70° C.) containing 5.3 kg of sodium chloride was gradually added.
温度は３５℃に保ち、滴下は６時間で終了した。The temperature was maintained at 35° C., and the dropping was completed in 6 hours.
その後、析出したＩＮ −ＧＮ混晶を遠心分離し、２８
．０Ｋｇの結晶を得た。Thereafter, the precipitated IN-GN mixed crystal was centrifuged and
．． 0 kg of crystals were obtained.
該結晶は厚みのある板状結晶であり、実施例１で得られ
たものと、流動性等の粉体特性においてほとんど同一で
あった。The crystals were thick, plate-shaped crystals, and were almost the same as those obtained in Example 1 in terms of powder properties such as fluidity.
［発明の効果］
以上説明したように、本発明によれば、厚みがあり、粒
径の大きくかつ流動性に優れたＩＮ −ＧＮ混晶が取得
できることから製造メリットが大きいものである。さら
に、本発明により製造された混晶はそのまま製品として
も適用できるものである。[Effects of the Invention] As explained above, according to the present invention, it is possible to obtain an IN-GN mixed crystal that is thick, has a large particle size, and has excellent fluidity, and therefore has great manufacturing merits. Furthermore, the mixed crystal produced according to the present invention can be used as a product as it is.
Claims (1)
−イノシン酸ジナトリウム含有溶解液を添加して混晶を
生成せしめるに際し、５’−イノシン酸ジナトリウムを
添加する前若しくは添加した後に、種晶として５’−イ
ノシン酸ジナトリウム結晶または５’−グアニル酸ジナ
トリウム・イノシン酸ジナトリウム混晶を添加せしめる
ことを特徴とする５’−グアニル酸ジナトリウム・５’
−イノシン酸ジナトリウム混晶の製造方法。Add 5' to the slurry solution containing disodium 5'-guanylate.
- When adding a disodium inosinate-containing solution to generate a mixed crystal, use 5'-disodium inosinate crystals or 5'-disodium crystals as seed crystals before or after adding 5'-disodium inosinate. 5'-Disodium guanylate/5' characterized by adding disodium guanylate/disodium inosinate mixed crystal
- Method for producing disodium inosinate mixed crystal.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1666390A JP2940044B2 (en) | 1990-01-27 | 1990-01-27 | Method for producing mixed crystals of 5'-disodium guanylate / 5'-disodium inosinate |
| DE4027360A DE4027360A1 (en) | 1989-09-04 | 1990-08-29 | Prepn. of mixed crystals of di:sodium 5'-guanylate and 5'-inosinate - the crystals have good flowing properties and are used as pharmaceuticals, esp. as condiments |
| KR1019900013583A KR0136902B1 (en) | 1989-09-04 | 1990-08-31 | Preparation process of crystal of mixture of 5'-guanylic acid disodium and 5'-inosinic acid disodium |
| BE9000852A BE1004566A4 (en) | 1989-09-04 | 1990-09-04 | Method for producing crystal mixed 5'-quanylate disodium and disodium 5'-inosinate. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1666390A JP2940044B2 (en) | 1990-01-27 | 1990-01-27 | Method for producing mixed crystals of 5'-disodium guanylate / 5'-disodium inosinate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03223299A true JPH03223299A (en) | 1991-10-02 |
| JP2940044B2 JP2940044B2 (en) | 1999-08-25 |
Family
ID=11922571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1666390A Expired - Lifetime JP2940044B2 (en) | 1989-09-04 | 1990-01-27 | Method for producing mixed crystals of 5'-disodium guanylate / 5'-disodium inosinate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2940044B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003011886A1 (en) * | 2001-07-26 | 2003-02-13 | Ajinomoto Co., Inc. | Method for producing mixed crystal of disodium 5'-guanylate and disodium 5'-inosinate |
| JP2003261594A (en) * | 2002-03-07 | 2003-09-19 | Kyowa Hakko Kogyo Co Ltd | Disodium 5'-xanthylate crystal |
| CN103570783A (en) * | 2013-11-19 | 2014-02-12 | 南京工业大学 | Crystal transformation method of disodium guanylate |
-
1990
- 1990-01-27 JP JP1666390A patent/JP2940044B2/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003011886A1 (en) * | 2001-07-26 | 2003-02-13 | Ajinomoto Co., Inc. | Method for producing mixed crystal of disodium 5'-guanylate and disodium 5'-inosinate |
| US7354615B2 (en) | 2001-07-26 | 2008-04-08 | Ajinomoto Co., Inc. | Method for producing mixed crystal of disodium 5′-guanylate and disodium 5′-inosinate |
| KR100866273B1 (en) * | 2001-07-26 | 2008-11-03 | 아지노모토 가부시키가이샤 | Method for producing mixed crystal of disodium 5'-guanylate and disodium 5'-inosinate |
| JP2003261594A (en) * | 2002-03-07 | 2003-09-19 | Kyowa Hakko Kogyo Co Ltd | Disodium 5'-xanthylate crystal |
| CN103570783A (en) * | 2013-11-19 | 2014-02-12 | 南京工业大学 | Crystal transformation method of disodium guanylate |
| CN103570783B (en) * | 2013-11-19 | 2016-08-17 | 南京工业大学 | A kind of Sodium guanylate turns brilliant method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2940044B2 (en) | 1999-08-25 |
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