JPH09235243A - Erythritol crystal and its production - Google Patents

Erythritol crystal and its production

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Publication number
JPH09235243A
JPH09235243A JP4444696A JP4444696A JPH09235243A JP H09235243 A JPH09235243 A JP H09235243A JP 4444696 A JP4444696 A JP 4444696A JP 4444696 A JP4444696 A JP 4444696A JP H09235243 A JPH09235243 A JP H09235243A
Authority
JP
Japan
Prior art keywords
erythritol
crystal
crystals
sieve
weight
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
Application number
JP4444696A
Other languages
Japanese (ja)
Inventor
Tsutomu Kondo
務 近藤
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 Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP4444696A priority Critical patent/JPH09235243A/en
Publication of JPH09235243A publication Critical patent/JPH09235243A/en
Pending legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

PROBLEM TO BE SOLVED: To produce a readily handleable erythritol powder, easily mixable with other food materials and having a smooth texture when eaten without consolidating by blending erythritol having a specific particle diameter in a prescribed proportion and reducing the moisture content in the powder to a prescribed value or below. SOLUTION: This erythritol crystal contains >=98wt.% crystal of 250μm undersize and <2wt.% crystal of 250μm oversize and has the moisture content thereof reduced to <=0.04wt.%. The erythritol crystal without consolidating is prepared by affording an erythritol crystal, containing >=97wt.% crystal having a particle size of 1000μm undersize to 360μm oversize and <3wt.% crystal of 360μm undersize and having the moisture content thereof reduced to <=2wt.% (in the first pulverizing and drying step) and further providing the erythritol crystal, containing >=98wt.% crystal of 250μm undersize and <2wt.% crystal of 250μm oversize and having the moisture content thereof reduced to s 0.04wt.% (in the second pulverizing and drying step). The second pulverizing and drying step is preferably carried out at 20-110 deg.C at <=65% relative humidity. The erythritol is useful as a sweetener.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は甘味料として有用な
エリスリトール及びその製造方法に存し、特にエリスリ
トール微粉末の保存に際して固結を抑制し使用時の粉砕
等が不要な容易使用可能なエリスリトール微粉末結晶及
びその製造方法に存する。
TECHNICAL FIELD The present invention relates to erythritol which is useful as a sweetener and a method for producing the same, and in particular, erythritol fine powder which is easy to use and which does not require crushing during use to prevent solidification during storage of erythritol fine powder. It exists in a powder crystal and a manufacturing method thereof.

【0002】[0002]

【従来の技術】甘味料として糖類、特に蔗糖は従来から
慣れ親しまれており、独特の甘味質からその消費量も多
い。しかし近年、蔗糖等の過剰摂取による虫歯、肥満、
糖尿病患者の増加などが問題になってきている。このた
め、製菓業界では蔗糖を含まない低カロリー、低う蝕化
を図った粉末糖が多数開発され、既に市販されているも
のもある。最近になって、四炭糖アルコールであるエリ
スリトールの製造方法が開発されて、エリスリトールが
低カロリー・非う蝕性甘味料として販売されたことか
ら、これを種々の甘味食品へ利用することが試みられて
いる。エリスリトールは四炭糖の糖アルコールで水溶性
に富み、非常に結晶化し易く、結晶は美麗で白色であ
る。甘味の強さは蔗糖の約75%であり、食すると爽や
かな冷感を感じるという特徴を有するのでテーブルシュ
ガー等に広く用いられてきた。また、エリスリトール微
細結晶粉末の外観は砂糖の粉糖の様で水に溶けやすく、
食した際冷感と滑らかな食感を有しているので打錠菓
子、ガム類及びチョコレート等様々な製菓製造に用いら
れている。例えば、特公昭56−18180号公報にエ
リスリトールを使用したチューイングガムなどへの利用
が記載されており、また特開平1−174332号公報
にはエリスリトールからなる非吸湿性アイシング剤に関
する記載がある。
2. Description of the Related Art Saccharides, particularly sucrose, have been used as sweeteners and their consumption is high due to their unique sweetness. However, in recent years, caries, obesity,
Increasing number of diabetic patients is becoming a problem. For this reason, in the confectionery industry, a large number of powdered sugars that do not contain sucrose and have low calories and low caries have been developed, and some of them are already commercially available. Recently, a method for producing erythritol, which is a four-carbon sugar alcohol, was developed, and erythritol was sold as a low-calorie, non-cariogenic sweetener. Have been. Erythritol is a sugar alcohol of tetracarbon sugar, is highly water-soluble, is very easily crystallized, and its crystals are beautiful and white. It has a sweetness of about 75% that of sucrose, and since it has a characteristic of feeling a refreshing cold sensation when eaten, it has been widely used for table sugar and the like. In addition, the appearance of erythritol fine crystal powder is easy to dissolve in water like sugar powdered sugar,
Since it has a cool and smooth texture when eaten, it has been used in the production of various confections such as tableted confectionery, gums and chocolate. For example, Japanese Patent Publication No. 56-18180 describes the use of erythritol in chewing gum and the like, and JP-A-1-174332 describes a non-hygroscopic icing agent composed of erythritol.

【0003】[0003]

【発明が解決しようとする課題】しかし、エリスリトー
ル粉末は蔗糖粉末に比較すると吸湿性が極めて小さいに
もかかわらず保存中に固結することがあり、使用に供す
る際に再度粉砕を必要とするなど取り扱いに不便な点が
あった。又、このような固結したものを用いると他の製
菓原料との混合に於いて混合が充分に行えず、例えば、
固結したエリスリトールを例えばチョコレートを製造す
る際ココアバター、ビターチョコレート、乳化剤などと
混合すると均一に混合することが出来ずグリツ状になり
肌理の滑らかなチョコレートは得られないという問題が
あった。
However, although erythritol powder has a very low hygroscopicity as compared with sucrose powder, it may solidify during storage, requiring re-grinding when used. There were inconveniences in handling. In addition, if such a solidified product is used, mixing with other confectionery ingredients cannot be performed sufficiently, for example,
When the consolidated erythritol is mixed with, for example, cocoa butter, bitter chocolate, an emulsifier or the like in the production of chocolate, there is a problem that the mixture cannot be uniformly mixed and becomes grit-like, so that chocolate having a smooth texture cannot be obtained.

【0004】[0004]

【課題を解決するための手段】本発明者は上述が如き問
題について鋭意検討した結果本発明を完成させた。本発
明者はエリスリトール結晶粒径1000μm篩下から3
60μm篩上が97重量%、水分0.05重量%のもの
を結晶粉砕し、粉末エリスリトールの水分を測定したと
ころ、以外にも水分量が2倍近く増加することが解っ
た。また、結晶粒径1000μm篩下から360μm篩
上の粒状結晶水分0.05重量%のものはクラフト袋に
入れ保存しても固結することがなかった。これら検討の
結果、エリスリトールの吸湿しにくい性質から、雰囲気
の湿度による影響で水分が増加することは殆ど無いの
で、固結原因はエリスリトール結晶間また結晶内部に存
在する水が粉砕によりフリーになることが原因であるこ
とが判明し、特定粒径のエリスリトールにおいて粉末中
水分量が0.04%以下であれば固結しないことが判明
し、本発明を完成させた。本発明は、固結しない粉末エ
リスリトール及びその製造方法を提供することを目的と
する。本発明は、250μm篩下の結晶を98重量%以
上、250μm篩上の結晶を2重量%未満含有し、水分
含有量が0.04重量%以下であることを特徴とするエ
リスリトール結晶に存する。
Means for Solving the Problems The inventor of the present invention has diligently studied the problems as described above and has completed the present invention. The present inventor has found that erythritol crystal grain size of 1000 μm
When the water content of the powder erythritol was measured by pulverizing the powder having 97% by weight on the 60 μm sieve and the water content of 0.05% by weight and observing the water content, it was found that the water content increased nearly twice. Further, those having a granular crystal water content of 0.05% by weight from a crystal grain size of 1000 μm under the sieve to 360 μm on the sieve did not congeal even when stored in a kraft bag. As a result of these examinations, since erythritol hardly absorbs moisture, moisture hardly increases due to the influence of the humidity of the atmosphere, and the cause of solidification is that water existing between erythritol crystals and inside the crystals becomes free by pulverization. It was found that the cause was that, and in erythritol having a specific particle size, if the water content in the powder was 0.04% or less, it did not solidify, and the present invention was completed. An object of the present invention is to provide a powdery erythritol which does not solidify and a method for producing the same. The present invention resides in erythritol crystals characterized by containing 98% by weight or more of crystals under a 250 μm sieve and less than 2% by weight of crystals on a 250 μm sieve and having a water content of 0.04% by weight or less.

【0005】従来よりエリスリトール結晶の乾燥方法は
通常流動乾燥で40〜50℃、10〜20分間行ってお
り、これで得られた結晶の水分は0.10%であるが内
部水分が除去出来ていないのでこれに内部水分を加えれ
ば約0.15〜0.20%と、固結するに十分な水が存
在することになる。(本発明における水分測定方法は常
圧105℃、4時間の加熱乾燥による蒸発減量を水分と
している)
Conventionally, erythritol crystals have been dried by fluidized drying at 40 to 50 ° C. for 10 to 20 minutes. The water content of the crystals thus obtained is 0.10%, but the internal water content can be removed. Since it is not present, if internal water is added to this, it is about 0.15 to 0.20%, which means that there is sufficient water for solidification. (The water content measuring method in the present invention uses the evaporation loss by heating at 105 ° C. for 4 hours as the water content)

【0006】結晶内部水分を除去する方法として高温長
時間乾燥する方法が考えられるが結晶内部の水は蒸発し
にくいし風味上からも臭いが付くなど好ましくない。こ
のような問題点に鑑み鋭意検討して成しえた本発明の今
一つの要旨は、エリスリトール結晶を1000μm篩下
から360μm篩上の結晶を97重量%以上、360μ
m篩下の結晶を3重量%未満含有し、水分含有量が0.
2重量%以下のエリスリトール結晶とする第一の粉砕乾
燥工程と、250μm篩下の結晶を98重量%以上、2
50μm篩上の結晶を2重量%未満含有し、水分含有量
が0.04重量%以下のエリスリトール結晶とする第二
の粉砕乾燥工程とを有するエリスリトール結晶の製造方
法に存する。
As a method of removing water inside the crystal, a method of drying at high temperature for a long time can be considered, but it is not preferable because water inside the crystal is hard to evaporate and smells from the flavor. Another gist of the present invention that has been made through intensive studies in view of such problems is that erythritol crystals from below 1000 μm sieve to above 360 μm sieve are 97 wt% or more, 360 μm or more.
m, containing less than 3% by weight of crystals under a sieve and a water content of 0.
2% by weight or less of the first pulverizing and drying step to obtain erythritol crystals, and 98% by weight or more of the crystals under the 250 μm sieve.
A second pulverizing and drying step of producing erythritol crystals containing less than 2% by weight of crystals on a 50 μm sieve and having a water content of 0.04% by weight or less.

【0007】[0007]

【発明の実施の形態】以下、本発明を詳細に説明する。
本発明のエリスリトール結晶は250μm篩下の結晶粒
子を98重量%以上含有するいわゆる微粉末であって
も、含水量を0.04重量%以下とすることで樹脂製袋
に梱包しても経時的な固結は生じず結晶は流動性を保
ち、製菓等の製造に際して有効である。含水分量が0.
04重量%を超えると梱包時は流動性を保っているもの
の、経時的に固結してしまう。
BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below.
The erythritol crystal of the present invention is a so-called fine powder containing 98% by weight or more of crystal particles under a 250 μm sieve, and even if it is packed in a resin bag with a water content of 0.04% by weight or less, It does not cause solidification, and the crystals remain fluid, which is effective in the production of confectionery and the like. Moisture content is 0.
If it exceeds 04% by weight, fluidity is maintained at the time of packaging, but it solidifies with time.

【0008】このような微細なエリスリトール結晶は通
常の方法で得られた結晶を任意の方法で粉砕・乾燥させ
て得られる。通常、エリスリトール結晶はブドウ糖等を
原料としてエリスリトール生産菌の存在下、水性培地
中、好気性条件下で培養して得た混合培養液を精製し、
これを晶析等の操作により回収される結晶を任意の方法
で粉砕・乾燥して得られる。中でも本発明の微細なエリ
スリトール結晶を得るには、エリスリトール結晶をま
ず、1000μm篩下から360μm篩上の結晶を97
重量%以上、360μm篩下の結晶を3重量%未満含有
し、水分含有量が0.2重量%以下のエリスリトール結
晶とし、次いでこの工程で得られた結晶を250μm篩
下の結晶を98重量%以上、250μm篩上の結晶を2
重量%未満含有し、水分含有量が0.04重量%以下の
エリスリトール結晶となるように粉砕乾燥する製造方法
に依るのが好ましい。
Such fine erythritol crystals can be obtained by pulverizing and drying the crystals obtained by a usual method by an arbitrary method. In general, erythritol crystals are purified from a mixed culture solution obtained by culturing under an aerobic condition in an aqueous medium in the presence of erythritol-producing bacteria using glucose as a raw material,
It is obtained by crushing and drying the crystals recovered by an operation such as crystallization by an arbitrary method. Among them, in order to obtain the fine erythritol crystals of the present invention, first, the erythritol crystals are first filtered from the bottom of the 1000 μm sieve to the crystals on the 360 μm sieve of 97.
Erythritol crystals containing less than 3% by weight of crystals under a sieve of 360 μm and having a water content of 0.2% by weight or less, and then the crystals obtained in this step are 98% by weight of crystals under a sieve of 250 μm. As above, 2 crystals on the 250 μm sieve
It is preferable to use a manufacturing method in which the content of the erythritol is less than 0.04% by weight and the erythritol crystals have a water content of 0.04% by weight or less.

【0009】このような粉砕乾燥工程を経ることで、固
結しないエリスリトール微細結晶が得られる。この工程
に於いて水分を除去する方法としては結晶を粉砕する
際、熱風又は乾燥空気を気流として用いる流動乾燥方法
で水を除去する方法が好ましい。乾燥空気の温度は高け
れば乾燥時間は短くなるが熱風温度は110℃を超える
とエリスリトールが溶解、溶融することがあるので11
0℃以下が好ましい。また、流動乾燥は相対湿度が低い
条件で行う方が良く、相対湿度を65%以下としておく
方が効率が上がり好ましい。乾燥方法は熱風を用いる棚
式乾燥機、トンネル型乾燥機等を用いることができるが
気流乾燥機は乾燥速度が早い、乾燥機と空気搬送装置の
機能をあわせもつので有利である。乾燥が終了したなら
ばエリスリトール結晶をポリエチレン等樹脂製袋に充填
し封をすることで固結が生じない。
Through such a pulverizing and drying step, erythritol fine crystals that do not solidify can be obtained. As a method of removing water in this step, a method of removing water by a fluidized drying method using hot air or dry air as an air stream when pulverizing crystals is preferable. If the temperature of the dry air is high, the drying time will be short, but if the hot air temperature exceeds 110 ° C, erythritol may melt and melt.
It is preferably 0 ° C or lower. Fluid drying is preferably performed under conditions of low relative humidity, and it is preferable to set the relative humidity to 65% or less because the efficiency increases. As a drying method, a shelf type dryer using hot air, a tunnel type dryer or the like can be used, but an airflow dryer is advantageous in that it has a high drying speed and has the functions of both a dryer and an air transfer device. When the drying is completed, erythritol crystals are filled in a resin bag such as polyethylene and sealed, so that no solidification occurs.

【0010】[0010]

【実施例】以下に示す実施例によって、本発明を更に具
体的に説明する。 実施例1及び比較例1〜2 表1に示す条件でエリスリトール(日研化学社製:粒度
分布は以下に記載)を以下の粉砕機を用いて粉砕した。
The present invention will be described in more detail with reference to the following examples. Example 1 and Comparative Examples 1 and 2 Erythritol (manufactured by Nikken Chemical Co., Ltd .: particle size distribution is described below) was pulverized under the conditions shown in Table 1 using the following pulverizer.

【0011】エリスリトールの粒度分布(単位:重量%) 1000μm篩上 0 1000μm篩下〜850μm篩上 3.3 850μm篩下〜710μm篩上 14.7 710μm篩下〜500μm篩上 67.4 500μm篩下〜360μm篩上 13.3 360μm篩下〜250μm篩上 1.3 250μm篩下〜180μm篩上 0 180μm篩下 0粉砕機 :ロータスピードミル P−14 フリッチュ社
製、スクリーンは梯形0.5mm、ロータ回転速度、1
4000rpm、試料フィダーとしてはSHINKO電
気社製C4−3型振動フィダーを用いた。
Particle size distribution of erythritol (unit:% by weight) 1000 μm on sieve 0 1000 μm on sieve-850 μm on sieve 3.3 850 μm on sieve-710 μm on sieve 14.7 710 μm on sieve-500 μm on sieve 67.4 500 μm on sieve 〜360 μm Sieve 13.3 360 μm Sieve 〜250 μm Sieve 1.3 250 μm Sieve 〜180 μm Sieve 0 180 μm Sieve 0 Crusher : Rotaspeed Mill P-14 Fritsch Co., screen is trapezoidal 0.5 mm, rotor Rotation speed, 1
At 4000 rpm, a C4-3 type vibration feeder manufactured by SHINKO Electric Co., Ltd. was used as a sample feeder.

【0012】粉砕条件及び粉砕後の粒径分布を表1に示
した。粉砕して得られたエリスリトール粉末30gをポ
リエチレン袋(6cm×6cm)に充填し、これに荷重
1500g(42g/cm2 )を乗せ、湿度RH79
%、温度20℃の条件下で7日間保存し固結状態を観察
・評価した。固結状態は丸型バネ式テンションゲージ
(OBA INSTRUMENT WORKS LT
D)で測定した。結果を表1に示した。
Table 1 shows the crushing conditions and the particle size distribution after crushing. 30 g of erythritol powder obtained by crushing was filled in a polyethylene bag (6 cm × 6 cm), and a load of 1500 g (42 g / cm 2 ) was placed on the bag, and the humidity was RH79.
%, The temperature was 20 ° C. for 7 days, and the solidified state was observed and evaluated. The solid state is a round spring tension gauge (OBA INSTRUMENT WORKS LT
D). The results are shown in Table 1.

【0013】[0013]

【表1】 [Table 1]

【0014】 *1 常圧、105℃、4時間の加熱乾燥による蒸発減量 *2 (テンションゲージ値) 0〜100 固結しない 101〜200 ゆるく固結 201〜300 固結 301〜500 固く固結* 1 Evaporative loss due to heating and drying at normal pressure, 105 ° C. for 4 hours * 2 (Tension gauge value) 0-100 No solidification 101-200 Loose solidification 201-300 Solidification 301-500 Solidification

【0015】実施例2−3及び比較例3〜4 以下の条件下、奈良式M−4型粉砕機(奈良機械社製)
を用い、実施例1と同一のエリスリトールを粉砕、乾燥
して得られたエリスリトール微粉末20kgをポリ袋に
充填し段ボール箱(縦、横、高さは各々31cm、45
cm、28cm)に入れて室温(10〜30℃)の条件
下1ヵ月間保存し固結状態を観察・評価した。結果を表
2に示した。
Examples 2-3 and Comparative Examples 3-4 Under the following conditions, a Nara type M-4 crusher (manufactured by Nara Machinery Co., Ltd.)
20 kg of erythritol fine powder obtained by crushing and drying the same erythritol as in Example 1 was filled in a plastic bag and the cardboard box (length, width, height was 31 cm, 45 respectively).
cm, 28 cm) and stored for 1 month under the condition of room temperature (10 to 30 ° C.), and the solidified state was observed and evaluated. The results are shown in Table 2.

【0016】粉砕条件 粉砕機 奈良機械(社)M−4型粉砕機、回転数3550(RPM)、スク リーン0.4、0.6(mm)、処理量(kg/min)20/2 乾燥温度 73℃ 粉体供給量 60(kg/H)、粉体投入方法 電磁フィーダ 室内雰囲気 26(℃)、RH70% Grinding conditions Grinding machine Nara Machinery Co., Ltd. M-4 type grinding machine, rotation speed 3550 (RPM), screen 0.4, 0.6 (mm), throughput (kg / min) 20/2 drying Temperature 73 ° C Powder supply rate 60 (kg / H), powder feeding method Electromagnetic feeder Indoor atmosphere 26 (° C), RH 70%

【0017】[0017]

【表2】 [Table 2]

【0018】[0018]

【発明の効果】以上詳しく説明した通り、この発明によ
って次のような効果が得られる。固結しないエリスリト
ール粉末は取扱いやすく他の食品材への混合が容易であ
りチョコレート、チューインガム、キャンデーなどに用
い、食した際ざらつきのない滑らかなものが得られる。
As described in detail above, the following effects can be obtained by the present invention. The non-caking erythritol powder is easy to handle, easy to mix with other food materials, and used in chocolate, chewing gum, candy, etc. to obtain a smooth product that is not rough when eaten.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 250μm篩下の結晶を98重量%以
上、250μm篩上の結晶を2重量%未満含有し、水分
含有量が0.04重量%以下であることを特徴とするエ
リスリトール結晶。
1. An erythritol crystal comprising 98% by weight or more of crystals under a 250 μm sieve, less than 2% by weight of crystals on a 250 μm sieve, and having a water content of 0.04% by weight or less.
【請求項2】 エリスリトール結晶を1000μm篩下
から360μm篩上の結晶を97重量%以上、360μ
m篩下の結晶を3重量%未満含有し、水分含有量が0.
2重量%以下のエリスリトール結晶とする第一の粉砕乾
燥工程と、250μm篩下の結晶を98重量%以上、2
50μm篩上の結晶を2重量%未満含有し、水分含有量
が0.04重量%以下のエリスリトール結晶とする第二
の粉砕乾燥工程とを有する請求項1に記載のエリスリト
ール結晶の製造方法。
2. Crystals of erythritol having a size of at least 97 wt.
m, containing less than 3% by weight of crystals under a sieve and a water content of 0.
2% by weight or less of the first pulverizing and drying step to obtain erythritol crystals, and 98% by weight or more of the crystals under the 250 μm sieve.
The method for producing erythritol crystals according to claim 1, further comprising a second pulverizing and drying step of forming erythritol crystals containing less than 2% by weight of crystals on a 50 μm sieve and having a water content of 0.04% by weight or less.
【請求項3】 第二の粉砕乾燥工程を20〜110℃、
相対湿度65%以下で行うことを特徴とする請求項2に
記載の製造方法。
3. The second crushing and drying step is performed at 20 to 110 ° C.
The method according to claim 2, wherein the method is performed at a relative humidity of 65% or less.
JP4444696A 1996-03-01 1996-03-01 Erythritol crystal and its production Pending JPH09235243A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4444696A JPH09235243A (en) 1996-03-01 1996-03-01 Erythritol crystal and its production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4444696A JPH09235243A (en) 1996-03-01 1996-03-01 Erythritol crystal and its production

Publications (1)

Publication Number Publication Date
JPH09235243A true JPH09235243A (en) 1997-09-09

Family

ID=12691725

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4444696A Pending JPH09235243A (en) 1996-03-01 1996-03-01 Erythritol crystal and its production

Country Status (1)

Country Link
JP (1) JPH09235243A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007070256A (en) * 2005-09-05 2007-03-22 Kao Corp Dentifrice composition

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007070256A (en) * 2005-09-05 2007-03-22 Kao Corp Dentifrice composition
JP4719537B2 (en) * 2005-09-05 2011-07-06 花王株式会社 Toothpaste composition

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