JP2671532B2 - Aspartame granules - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION Industrial Field of the Invention The present invention provides aspartame with improved solubility (α-
L-aspartyl-L-phenylalanine methyl ester) granules.

(Prior Art) Aspartame is widely used as a low-calorie sweetener because it has a bitterness and aftertaste that are generally found in high-intensity sweeteners and has a refreshing sweetness. However, aspartame is physically dispersed in water. However, it has been pointed out that the solubility is low, and conventionally, in order to obtain aspartame having excellent solubility, granulation with addition of an excipient and a disintegrant, effervescent tableting and the like have been studied. However, there are many cases where mixing of excipients and the like becomes a problem depending on the application, and there is a strong demand for aspartame having high purity and good solubility.

As attempts to improve the solubility of aspartame while maintaining high purity, a method of spray-drying aspartame in a slurry state (Japanese Patent Publication No. 58-20588) and a method of granulating aspartame hydrolyzed to a specific water content (Japanese Patent Application Laid-Open No. 59−9586
2) and the like. Regarding the solubility of the aspartame crystals themselves, see II A, I in JP-A-59-172444.
The IB-type crystals have better solubility as dry crystals than the IB-type crystals, but the solubility of II A, II B-type crystals, especially II B-type crystals, is low, and it is long for dispersion and dissolution in water. It takes time.

(Problems to be Solved by the Invention) The present invention aims to improve the solubility of the above-mentioned type II crystal.

(Means for Solving the Problem) The inventors of the present invention have conducted extensive studies to solve the above problems, and as a result, the solubility is improved when the aspartame type II crystal is granulated to have a specific particle size. The inventors have found that and completed the present invention.

Aspartame II type B crystal in the present invention means Cuk α
At least when measured by powder X-ray diffractometry using X-ray
X-ray diffraction at diffraction angles of 15.2 °, 11.1 °, 19.6 ° and 4.5 °
It is a crystal that shows the peak of the X-ray, and aspartame II A-type crystal is a diffraction angle of at least 20.6 °, 21.2 °, 5.0 ° and 11.1 ° when measured by powder X-ray diffraction method using Cuk α-ray. It is a crystal showing an X-ray peak.

When granulating and molding using a binder, the binder is appropriately selected from water, alcohol, saccharides and aqueous solutions of inorganic substances.

The method for producing the granules may be any of mixed granulation, pressure granulation, extrusion granulation, fluidized granulation, tumbling granulation, crushing granulation, etc. In order to avoid the complexity of the process, it is industrially advantageous to use dry granulation such as pressure granulation.

The particle size of the granulated product needs to be in the range of 150 to 1400 μm, preferably 180 to 500 μm. If the particle size is smaller than 150 μm, the dispersibility in water is poor and it takes a long time to dissolve. On the contrary, if the particle size exceeds 1400 μm, the contact area between the particle and water decreases, which is not preferable. Therefore, the particle size of the granulated product is 150-1
400 μm, and within this range, aspartame II
The time required for dissolving the crystal in water can be reduced to about 1/3 to 1/10.

Example (Production of Sample) Sample A: According to a conventional method, after stirring and crystallizing accompanied by stirring of an aspartame aqueous solution during cooling crystallization, centrifugal separation was performed to obtain a wet aspartame crystal having a water content of 50% by a screw feeder. Continuously feed it to a micron dryer (made by Hosokawa Micron), dry it with airflow at a hot air inlet temperature of 135 ° C, and then load it into a small vacuum dryer for the laboratory.
It was vacuum dried at 120 ° C. for 6 hours to obtain aspartame II type B crystal.

Sample B: Raw material aqueous solution 380 L (55 ° C, initial concentration of aspartame of 4.4) with 17.7 kg of aspartame dissolved in a stainless steel crystallizer with a jacket and a cooling plate inside and having a diameter of 400 mm.
% By weight), and a refrigerant having a temperature of 0 ° C. was circulated through the jacket and the cooling plate and cooled for 3 hours. After about 1 hour, the entire solution became a pseudo solid phase. This pseudo solid aspartame crystal is dropped into a receiving tank equipped with a cooling coil and a stirrer,
It was crushed, slurried, and cooled (cooled from 16 ° C to 7 ° C in the receiving tank). The slurry obtained in this way has a diameter of
When dewatering was performed by a 36-inch centrifuge, wet crystals of aspartame having a water content of 30% were obtained.
Wet crystals of aspartame obtained by such a static crystallization method were continuously fed to a micron dryer (manufactured by Hosokawa Micron) by a screw feeder, and air-dried at a hot air inlet temperature of 135 ° C for further laboratory use. The mixture was placed in a small vacuum dryer and vacuum dried at 120 ° C. for 6 hours to obtain aspartame II type B crystal. It was dried at 120 ° C. for 6 hours to obtain aspartame II type B crystal.

Sample C: According to a conventional method, after stirring and crystallization accompanied by stirring of the aspartame aqueous solution during cooling and crystallization, centrifugally separated wet crystals of aspartame with a water content of 60% were continuously fed with a screw feeder to a micron dryer (Hosokawa Micron). Product) and air-flow dried at a hot air inlet temperature of 140 ° C.
An IA type crystal was obtained.

Sample D: According to the usual method, after stirring and crystallization accompanied by stirring of the aspartame aqueous solution during cooling and crystallization, centrifuge the separated wet crystals of aspartame with a water content of 60% were put into a small laboratory fluidized dryer. The crystals were dried at 90 ° C for 30 minutes to obtain IB type crystals.

Sample E: A mixture of equal amounts of the IB type crystal (Sample D), the II A type crystal (Sample C) and the II B type crystal (Sample A) obtained above.

Each of the samples obtained above was compression-molded under the following conditions to obtain pressed flakes, and then crushed with an oscillator to obtain aspartame granules having a particle size shown in Table 1.

Table 1 shows the dissolution time of the obtained aspartame granules. The dissolution time was measured by the following method.

Pour 2 L of water into a 3 L beaker and stir using a magnetic stirrer. The size of the rotor is 70 mm x 15 mmφ, and the rotation speed is 350 rpm using Whatman Dataplate 440.
And keep the water temperature at 20 ° C using the hot plate function. After adding 8 g of the sample, measure the time until it is completely dissolved.

(Conditions for compression molding and crushing) Using a roller compactor model mini (manufactured by Freund Sangyo), dry compression molding and crushing were performed under the following conditions.

・ Volume of raw powder: 50g / min. ・ Roll pressure: 60kg / cm ²・ G ・ Roll speed: 4rpm ・ Oscillator (crusher) wire mesh: 12 mesh screen * 12 mesh opening: 1400μm (Effect of the Invention) According to the present invention, the dissolution time of aspartame type II crystal, which has conventionally been poor in solubility and has a problem in use in beverages and the like, is significantly shortened, and practicability in beverages and the like is obtained. In particular, when the II B type crystal is contained alone or mixed with another crystal type such as II A, the solubility improving effect is high.

 ─────────────────────────────────────────────────── --Continued from the front page (56) Reference JP-A-2-174650 (JP, A) JP-A-60-37949 (JP, A) JP-A-59-172444 (JP, A) JP-A-59- 95862 (JP, A)

Claims (2)

(57) [Claims] 1. Aspartame II type A crystal and / or II B
An aspartame granule containing a shaped crystal and having a particle size in the range of 150 to 1400 μm. 2. The aspartame granules according to claim 1, which have a particle size in the range of 180 to 500 μm.