AU592346B2 - Sugar cubes containing aspartame - Google Patents

Description

AUSTRALIA 5 2 4 Patents Act COMPLETE SPECIFICATIOU

(ORIGINAL)

Application Number: Lodged: Clasls Int. Class Compl3ete Specification Lcrdged: Accepted: Published: Priority Related 1:rt: t t It C C CC 0C t C APPLICANT'S REFERENCE: DD/LP 9312B/88 Name(..) of Applicant(s): LABORATOIRES POLIVE-NUHRLIN SA Address(es) of Applicant(s): 19-23 bd G Clemenceau F-92400 Courbevoie France Address for Service i0: PHILLIPS ORMON3E FIIZZPATRICK Patent and Trade Mark Attornevs 367 Collins Street Melbourne 3000 AUSTRALIA Complete Specification 'dor the invention entitled: PROCESS OF INCORPORATION OF A HYGROSCOPIC AID LOW SOLUBILITY SUBSTANCE, ESPECIALLY ASPARTAME, IN V'OOD PRODWI-TS CONTAINING SUGAR The following statement is a full description of this invention, including the best method of performing it known to applicant(s): 11 1) 77j7 -2 PROCESS OF INCORPORATION OF A HYGROSCOPIC AND LOW SOLUBILITY SUBSTANCE, ESPECIALLY ASPARTAME, IN FOOD PRODUCTS CONTAINING SUGAR The invention concerns food products of which sugar is the main component, and relates to a process permitting to izncorporate in this product a substance such as aspartame or any other substance presenting similar physico-chemical properties, especially its hygroscopic characteristic existing along with a low solubility, while guaranteeing an homogeneous result.

~ii *t Aspartame, abbreviated APM, is a very good sweetener with a profile similar to that of sugar. It is an organic product of structure C4 H18 N2 05, MW (Molecular Weight) 294

NH

S- CH2 CH NH CO O C CH CH COOH I 2

O

itre

C

CO

I ICL

I

CH 3

NH

2 Its sweetening capacity, 180 to 200 times that of sucrose, causes it to be sought as a substitute for the latter, from the dietetic point of view.

However, some of its properties may limit its capabilities of incorporation into food products.

It is strongly hygroscopic and its water solubility is low, varying with pH and temperature. For a pH between 4 and 5, where it is the most stable, the solubility is 3% at 0.7% at 20°C; so that 100 liters of water are necessary to solubilize 700 g of APM equivalent to 126 kg of sweetening capacity expressed in saccharose.

3 Its stability is poor when the pH is very acid or very alkaline.

Its high sweetening capacity makes the dosage delicate; it must, however, remain accurate.

It becomes sticky in humid environment and its tendency to agglomerate, even in powdery form, is obvious.

Consequently, these drawbacks cause great difficulties ofi practical implementing in alimentary applications, especially when it concerns molded products.

As a matter of fact, these food products are initially presented in the form of powders in which one may try to incorporate directly a quantity of APM precisely titrated.

j But this is a delicate procedure and a source of many difficulties: a formation of aerosols, difficult homogeneous distribution and sticking at the time of a subsequent introduction of water in limited quantity.

It was then attempted to prepare a solution or a suspension of APM in pure water subsequently diluted in a solid powder, sugar for instance. But a solution of low concentration is obtained because of the large quantity of Oc" water necessary to insure acomplete solubilization or, in the case of a suspension, it is a sticky putty, impossible to handle and preventing any subsequent use.

00' The invention concerns a proceduie permitting to S*incorporate easily aspartame or any other substance with similar physico-chemioal properties, into a molded food product containing crystallized sugar, and by which the problems mentioned above are eliminated and guarantee an homogeneous distribution of APM.

According to the 1 .nvention, the procedure consists in preparing an homogeneous suspension of the substance into a 4 M'i r 1 -4concentrated sugar syrup, in mixing this suspension with the aforesaid food substance containing crystallized sugar and molding the mixture obtained; the amount of water necessary for molding comes essentially from sugar syrup and titration of the substance in the suspension being determined in function of its titration in the sugar pieces.

The term sugar relates to any classical mono or (isaccharide as well as their mixture. The sugar in the syrup may be different from the crystallized sugar in the alimentary product.

The sugar in the syrup may be especially selected among saccharose, glucose, inverted sugar and lactose, and for the crystallized sugar among saccharose or fructose.

;tt As a matter of fact, it has been established that when APM is placed in suspension in solutions of increasing S titres of saccharose in water, one obtains suspensions more and more stable and easy to handle and able to be perfectly weighed, pumped, diluted and incorporated to other products, when the Brix rises. This is valid for a quantity of APM Snot exceeding 40% of the syrup mass.

This phenomenon depends directly r)n the quantity of t water available in the solution and nonbound to the sugar.

c'm Especially for saccharose, at the limit of its solubility in water,, at 66.6 Brix, there is no longer free water and S; practically all the molecules of water are associated to the c~G sugar molecules.

A It is actually established that the solubility of APM in a sugar solution decreases with the increase in sugar concentration. At 40°C for instance, the solubility of APM is: 1.3% in pure water 0.7% in a saccharose solution at 40 Brix 0.4% in a Saccharose solution at 60 Brix I: I 5 In addition the chemical stability of APM in a solution of sugar or of inverted sugar is improved with the Brix increase. Refer to the article by M. PRUDEL and E.

DAVIDKOVA in the Review DIE NAHRUNG (Volume 25 of February 1981, Pages 193-199) which demonstrates the favourable influence of this factor, mostly when the Brix is high: at Brix, the stability (expressed in half-life time) is 1.7 times stronger than in water, under equivalent conditions of temperature and pH. This fact has been confirmed and no apparent degradation was noticed in 50 h at 40 0 C, in saccharose solutions of 60 Brix at pH 6. The same is true in solutions of inverted sugar.

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4* .4 6 4; 4. 6 4140 Sr *4Q4t .44, As for every sugar solution, it is advisable to take all necessay precautions in order to avoid or reduce bacterial contaminations. One should always try to have the lowest possible hydric water activity (WA).

The mechanical stability of an APM suspension in a sugar solution is not constant in time, mostly at low Brix: it varies between a few minutes and 8 days (60 Brix for saccharose) at the end of which there is a beginning of decantation of the dispersion. If it becomes necessay to keep such suspensions for a long time, the adjunction of gums (xanthanes, for instance) is sufficient to insure that the medium has an adequate viscosity to avoid any phenomenon of separation and decantation. Doses 0.1% of xanthanes are sufficient for syrups of 40 Brix and over. Also, any soluble additive may be added to the water of the syrup.

The procedure, according to the invention, is therefore divided in three steps: the first one is the essential step, consisting in the preparation of a premi' the second step consists in mixing this premix with the food product made with crystallized sugar; the third step consists in molding the mixture obtained.

St« I Q\ f S.;BO0 1 6 The premix is prepared as follows: a solution or a concentrated sugar syrup is prepared; the concentration of sugar in the syrup is preferably between 60% and 100% of its saturation, which, for saccharose, corresponds to an interval between 40 and 66 Brix at 20 0

C.

the substance, APM under the circumstances, is introduced, in powder form, and dispersed by any manual or mechanical means of stirring and distribution, in order to obtain a premix in the form of a suspension of this substance in the syrup.

In this premix, the quantities in question of the S. substance, of water, and therefore of syrup, are directly related to the final composition of the desired product.

S Generally, the quantity of the substance in question must be, at most, equal to 40% of the syrup mass.

If necessary, the dispersion is completed with an intense mechanical treatment, using a grinder with rings S (stephan) or any other similar device, checking an eventual temperature elevation. This treatment reduces the aggregates of the substance formed in contact with a liquid Smedium, into simple particles. It is noticed that, in the I"Z syrup, aggregates do not re-form.

S- Thus, a premix is obtained ir the form of a stable, Sicr homogeneous suspension, more or less thick and viscous, U it which may be subseqlently diluted int' a powder.

Other products may be incorporated to the sugar syrup, such as coloring agents, flavourings, various additives, solubles or non-soluble in water or syrup in order to manufacture complex premixes.

C 7 In the same way, a mixture of sugar inverted may be used. In the same way, addition of a bacteriostatic agent (sorbate for instance), contributes to stabilize the premix for stocking.

In the same way, it is possible to add solubilizing mineral agents of APM, type acid sulfate of sodium or potassium, as they appear in the European Patent 0109685.

In the second stage, the premix is incorporated to the mass of food product containing crystallized sugar, in an appropriate mechanical mixer, guaranteeing a distribution while avoiding the erosion of sugar crystals.

S The last step of the procedure consists in molding the mixture thus obtained in the form of pieces. The necessary I quantity of water is provided by the premix itself, and for this operation groups of molding-drying, type Chambon, or SS l any other classic technique of sugar-refinery, may be used.

The following examples, relating to aspartame, illustrate the incorporation method.

t a) Preparation of a premix made of sugar and aspartame ocn c e In a planet mixer, 4.920 kg of APM are introduced and Sct 20.08 kg of a saccharose syrup at 65.5 Brix are poured in a trickle. After absorption and coarse manual mixing, a good Ci dispersion is insured by mechanical stirring for 15 minutes.

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This mixture is transferred in a recycling grinder, Stype MICROCUT STEPHAN, in which it is treated for 3 minutes at a temperature not exceeding 40 0 C. A subsequent microscopical examination confirms that the aggregates are no longer present. The premix thus obtained is stocked in a closed container. In two samples taken an- analyzed by HPLC (spectro at 257 mm), the following results for APM content

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Q o f a~ R~iI 8 are found: Theoretical Sample 1 Sample 2 19.68% 19.64% 19.29% b) Preparation of low calories mini sugar pieces The synergy between sucrose and APM is a known phenomenon. Within the scope of the research for new products of low caloric capacity, to be offered to consumers for health or dietetic reasons, sugar cubes of small size are proposed, containing 0.5 to 2% APM and guaranteeing for the user an absorbed energy of about 20 to 50% of that he S should hav i -,gested in a sugar form to have the same S sweetening ;i acity. These products are in essence different from the tablets already existing on the market.

t «t *a This procedure has been applied to the preparation of sugar in lump form according 4-o the assic technique of sugar molders, i.e. molding t a sugar of given granulometry, with a humidity between 0.8 and 1.1 and in general.

The premix prepared in a) is incorporated in 300 kg of crystallized sugar, premium quality, with a granulometry identical to that used for the molding of classic lumps.

The apparatus is an inox vertical mixing machine with stirring provided by a mechanical arm at the bottom of the tank and a volume of 500 liters. The sugar is loaded with an automatic scale and the premix barrel is carefully emptied. Mixing is carried out for 15 minutes at a temperature not exceeding 40 0 C. The solid product thus obtained is able to be molded directly on a classic molding set. It may also be stocked in a watertight container for subsequent use without any special problem of lumping, The product thus obtaining corresponds to the following 3, 0't i 9 1 analysis: Sugar 96.64 APM 1.38 1.98 100.00 In 2 samples, the APM content is 1.32% and 1.33% and the quantity of water introduced through the sugar syrup corresponds to the needs of the molding.

Therefore, the preparation of this mixture permits, very easily, to adjust exactly with the method advocated, the content of each component by modifying the Brix and the quantity of syrup.

Tre mixture thus obtained is molded on a classic molding set in refinery equipped with molding plates of I**r Srequired dimensions, 15 x 11 x 6 mm in this case (adjustable thickness) and delivering sugars of an average weight of 2 1.1 g. After classic molding and baking, the average theoretical composition of the sugars is: s I Sugar 98.34 APM 1.41 0.25 (measured experimentally) 100.00 or for a "minisugar" of 1.1 g, a dosage of 15.47 mg of APM.

C C CThe statistical distribution of the weights of the ,P tAP9 "mirisugars" is identical to that of a normal molding set as well as the rhythm of the machine, which means that the S mixture does not behave differently than a pure humid sugar.

Titrations of APM were done on a series of pieces (sugar) in order to verify the good distribution of the active principle.

I -1 1"U"10 1 1 111 1 1 11f^^

I

i 1 10 In 20 pieces, individually titrated, the mean APM dosage is 1.35% 0.03 which gives a standard relative deviation of 2.22%.

The losses observed correspond to the normal losses in the manufacturing process; losses from dragging solid APM dust, losses during decanting, losses in the machine. The search for dicetopiperazine, main degradation product of APM, always showed to be negative, in all stages of the procedure.

c) Preparation of sugar cubes with reinforced sweetening capacity *i S i t I t I I C Ir C II C1 U C I I0 ;tII I Ic ii I Returning to the mode of operation a premix was prepared with the following ingredients: Sugar syrup at 65.3 Brix 21.87 kg APM 7.40 kg The theoretical composition of the premix is: Sugar 48.79 APM 25.29 H2O 25.92 100.00 According to the mode of operation 25.7 kg were taken from this prelnix and incorporated to 300 kg of sugar for molding.

The molding mixture had the following theoretical composition: Sugar 95.96 APM 2.00

H

2 0 2.04 100.00 The mixture is molded in cubes corresponding to a No. 6 size (dimensions 27.5 x 17.5 x 11, adjustable thickness).

11 After baking, the moisture, measured experimentally, is 0.45%. The average composition of the sugars is: Sugar 97.52 APM 2.03 0.45 (measured) 100.00 The quality of the production was tested on several series of 20 cubes, analyzed individually. The results from a series of 20 cubes for a given compression, are given below: in terms of regularity of the weight of the cubes mean weight 3.53 g 0.09, or a standard relative deviation of 2,55%.

in terms of APM content mean content 1.87% 0.04, or a standard relative deviation of 2.14%.

These values confirm a satisfactory distribution of the a f unit weight of the cubes as well as the good distribution of APM in the mixture for molding. Nevertheless, a difference remains between the measured APM content and the theoretical content This difference is not due to S' a degradation of APM, since the total absence of S dicetopiperazine in these products was verified. It is explained, in addition to the manufacturing losses, by a S systematic shifting by default of the method of dosage used.

Taking into account the absence of any secondary S product, the proposed method enables to provide products in which APM is regularly distributed. The molding method insuring constant individual weights, such experimental conditions may be predicted that it is possible to guarantee the weight of constant active principles in sugar cubes.

1 12 Especially, it is possible to guarantee a concentration sufficiently constant and accurate, so that this dispersion method may be used to distribute active principles in sugar cubes in guaranteeing a given dose an active principle for each sugar cube. Thus, it is contemplated to propose a new form of medication support.

d) Preparation of sugar cubes permitting the production of a lemon-flavoured hypocaloric drink According to a) a concentrated premiv. of lemon drink is prepared.

In a planet mixer or inox equivalent, are placed 101.2 g of APM; 298.89 g of syrup at 65.3 Brix are poured in, mixed gently at low speed to start then in second gear to complete the homogenization.

This premix is then put through a ring grinder in order to tear the APM aggregates formed in contact with the s" yrup. This premix is preserved for subsequent use.

In a mixer with stirrer at the 'mottom of the tank, the following products are loaded; refined powdered sugar 150 g t maltodextrins 54 g pturified, strained gum-arabic 59 g ascorbi4 acid I g I j 0 citric acid 25 q Dry-mix for 3 ninutes at slow speed. In addiition, mix n t' coarsely but extnmporaneously in a container wh:lch will be o. completely emptied in the powdery nmx: premix prepared as above synthetic lemon flavour, kypa "Firmenich 51124A"

C

2L ~-prane -rrram~ Everything is mixed together for 3 mi.nutes at slow speed: the complement of refined powdered sugar is added A total load of 150 477 q is obtained.

Mix for 3 minutes at low speed, then for 10 high speed.

minutes at An homogeneous mix, in which constituents are evenly distributed, is The comnposition of the mix is powdered sugar maltodextrins purified gum-arabic ascorbic acid citric acid synthetic lemon flavour "Firnenich 51124A" water

APM

APM and obtained.

the other

II

I 4 44 44 4

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II 4 4i 4 4 44d 46 4 '4 44 *t 4 44 444 44CL 4PC) 66.47% 11.32% 12.37% 0.21% 5.24% 0.63% 1.90% 1,86% 100.00% Finaly, this mix is molded according to the usual technique used in sugar-refinery to obtain cubes of about 5 g.

Two cubes in 150 ml of water make a pleasant drink.

The final drink has the following characteristics for 100 ml: caloric capacity 10.63 Kcal (in comparison 100 ml of "Coca Cola Light" 5 Kcal).

sweetening capacity 16.00 g of saccharose equivalent.

pH 2.90 (correspording to a pH of j good APM stability).

1

I

14 Colouring agents may also be added to the syrup or to the dry mix depending on their water solubility.

The method permits to prepare, in the form of a sugar cube, an homogeneous mix used as a self-prepared drink which may be packaged individually for a given dose.

Manufacture of a light drink is thus easily realized.

The following example resumes this application while improving it.

e) Sugar cubes as flavouring supports for a preparation of a light, instant, sparkling drink Preparation of a premix In a planet mixer or inox equivalent, 180 g of APM are placed and 520 g of cold sugar syrup at 65.3 Brix are poured over it in a trickle; mix gently in first gear to start, then in second gear to complete the homogenization.

This premix is then put through a ring grinder in order to tear the small APM aggregates formed in contact with the syrup.

Preparation of the mix In a mixer with inox stirrer the following solid ingredients: *s tv et t t4 C id 4 4r

I

71 4C r

CC

OC~

sugar with granulometry adapted to the molding (Sugar A) citric acid xanthane gum pu ified, strained gum-arabic sodium bicarbonate 300 g 55.5 g 7.4 g 7.4 g 18,2 g 4.q.ZUL Dry-mnix for 3 minutes.

4( t//0 t 0 I r Ar-~ In addition, mix closely and extemporaneously the following ingredients (at a temperature of 20 to 25 0

C):

-premix 65.4 g "Riboflavine Roche" (vit. B2) 0.6 g synthetic lemon flavoured "Firmenich 51.24A" 3.7 q 69.7 g This mixture is completely emptied into the powdery mix; it is mixed for 3 minutes, then 300 g of sugar A are added and mixed for 3 minutes in first gear and 10 minutes in second gear.

The mixture may 'e molded on a classic molding set of refinery (size 6) (unit weight 3.4 g).

r t C 1 26 ci After molding, the sugars undergo baking at a temperature lower than that normally used (60°-70 0 not exceeding 40 0 C to prevent washing down of the flavouring, which is very vol tile.

Baking will be in fact adjusted to the quaiity and the characteristics of the flavourings used in this type of procedure.

C I t t~ c r c f r p cn0 r,- C I t I The composition of a following: sugar

APM

-"Riboflavine" lemon flavour -citric acid -xanthane gum gum-arabic -sodium bicarbonate -sugar syru 65.3 B total sugar 2.8332 sugar cube of 3.4 g is the 2.6911 g 79.15% 0.0750 g 2.21% 0.0027 g 0.08% 0.0166 g 0.49% 0.2490 g 7.32% 0.0330 g 0.97% 1,0330 g 0.97% 0.0820 g 2.41% 0.2176 g 6.40% 83.33% :f 16 Introduced in a glass containing 100 ml of cold water, the release of CO 2 helps the dissolution of the sugar cube. However complete dissolution is obtained by stirring with a spoon.

100 ml of the final drink have a caloric capacity of 11.3 Kcal and a sweetening capacity equivalent to 16.33 g of saccharose.

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Claims (9)

1. A process for the production of a food product based on granulated sugar which is in the form of shaped pieces and contains a substance of low solubility in water, said process comprising; preparing a homogeneous suspension of the said substance in a sugar syrup the concentration of which is between 60% and 100% of saturation, mixing this suspension with granulated sugar and finally shaping said mixture into pieces and drying.

2. A process according to Claim 1, wherein the quantity of said substance is at most equal to 40% of the mass of syrup.

3. A process according to Claim 1 or 2, wherein the suspension is subjected to a mechanical treatment intended to reduce the aggregates of the substance which may have been formed during its incorporation. 9

4. A process according to any one of the preceding claims, t i at wherein the at least one additive selected from the group: S colorant, flavouring, bacteriostatic agent, inorganic solubilizing agent of the said substance and gum, is incorporated into the syrup. t" t 5. A process according to any one of the preceding claims, ",EI wherein the sugar constituting the syrup is selected from at least one of the following: sucrose, glucose, invert sugar and lactose.

6. A process a c.ording to any one of the preceding claims, 4 wherein the granulated sugar is sucrose or fructose.

7. A process according to any one of Claims 1 to wherein the shaped food product is a mixture for a fruit flavour drink to be prepared by the user, the said flavouring being incorporated in the suspension. molding the mixture obtained. "W ,f 18

8. A process according to any one of the preceding claims, wherein said substance comprises between 0.5% and 2% of aspartame.

9. A process according to Claim 1 substantially as hereinbefore described with reference to any one of the examples. A food product when prepared by the process of any one of Claims 1 to 9. DATED: 17 October 1989 PHILLIPS ORMONDE FITZPATRICK Attorneys For: LABORATOIRES POLIVE-WtIHRLIN SA eW w t r r «O ttC I et e C t c f t CI t t 4 t f r 64t t t e i 46I? i t 4 5786h ~1~J INTERNATIONAL SEARCH REPORT International Application No PCT/FR86/00158 -I I. CLASSIFICATION OF SUBJECT MATTER (if several classification symbols soply, Indicate all) According to Intenationl Patent Classification (IPC) or to both National Classification and IPC Int.Cl. C 13 F 3/00; C 13 F 3/02; A 23 L 1/236;A 23 L 1/09 II. FIELDS SEARCHED Minimum Documentation Searched 7 Classification System Classification Symbols IntCl4 C 13 F In A 23 L Documentation Searched other than Minimum Documentation to the Extent that such Documents are Included In the Fields Searched Ill. DOCUMENTS CONSIDERED TO BE RIELVANT'_ Category I Citation of Document, with Indication, where appropriate, of the relevant passages t I Relevant to Claim No. 13 X EP, A, 0102032 (AYINOMOTO CO.INC) 7 March 1984, see claims 1-8; page 9, line 24 page 1 3,4,5,6 line 2; page 10, line 23 page 11, line 9; page 13, lines 23-26; page 15, lines examples 1,3 A EP, A, 0109771 (GENERAL FOOD CORPORATION) May 1984, see claims 1,4 1-6 A EP, A, 0106910 (AJINOMOTO CO.) 2 May 1984, see claims 1-5 1-11 A FR, A, 2245299 (GENERAL FOOD CORPORATION) April 1975, see claims 1,2; examples 1,3 1-11 Special categories of cited documents: s later document published after the international filing date A" docum <nt dfining the gnrl state o thei art which is not O pri'lority date and not In conflict with the applicatlon but S cuntd te ee tte o the art hich not cited t understand the principle or theory underlying the considered to be of polcular relevance invention "E l earlierdocument but published on o r ter the international X" document of particular relevance; the claimed Invention filng date cannot be considered novel or cannot be considered to document which may throw doubts on priority claim(s) or Involve an inventive step which Is cited to establish the publication date of another document of parliculir relevance; the claimed Invention citation or other spoclial reason (as specified) cannot be considered to involve en Inventlve stp when tho document referring to an oral disclosure, use, eihibition or document is combined with one or more other such docu. other means ments, such combination being obvious to a person skilled document published prior to the International filing date but In the art. later than the priority date claimed dcument member of the sam patent family IV. CERTIFICATION Date of the Actual Completion of the International Search Dt of Mailing of this International Search Report 4 August 1986 (04.08.86) 27 August 1986 (27.08.86) Internationl Searching Authority Signature of Authorlled Officer European Patent Office Form PCTIISA/210 (second shoet) (January IHs) 51 ^irW-ti ANNEX TO THE INTERNATIONAL SEARCH REPORT ON INTERNATIONAL APPLICATION NO. PCT./FR 86/0015& (SA 13154) This Annex lists the patent family members relating to the patent documents cited in, the above-mentioned international search report. The members are as contained in the European Patent Office EDP file on 13/08/86 The European Patent Office is in no way liable for these particulars which are merely given for the purpose of information. Patent dopument .Publicati-'on. Patent family Publication cited in .Search date member(s) date report EP-A- 0102032 07/03/84 jP-A-: 59031669- 20/02/84 JP-A- 59031656- 20/02/84 EP-A- 010977f1 -'330,205/84 Non'e EP-A- 0106910 02/0-5/84-C None FR-A- 2245299 J ?5/04/.75- No0ne. 14 4. se efficia Jora ol the 4.~p~nPaetOf o 28 RAPPORT DE RECHERCHE INTERNATIONALE Demands International* N, PCT/ FR 86 /00 158 1. CLASSIMINT 01 LINVENTION piusiours symcoles do Classification sont PPlcnbies, (as Indiquor tous) Solon In classification International@ des brevets (cm9 oQ A is tois salon In classification national* at I& ClB IB 4 C 13 F 3/00; C 13 IF :3/02; A 23,L 1/236; A 23 L 1/09 It. 'JOMAINKS SUR LISQUILS LA RE111CHINCHE1 A 11101111T1 Documentation minimai. consulie a Systbm* do classification Symbolies do clasiicationl CI 4 C 13 F CI A 23 L Documentation consulit. sutre quo Is documientation minimalie dana as mesure o4i do lte documents font panis dos domalnts sun sequois to recherche a porA

111. OCCUMNTS CONSloj111111 COMMI PERTININTS Catilgorie *Identification des documents citsil avec Indication, si niceasaire, N, des revendiceations, des passages pertinents Is W1 vis' X EP,, A, 010,2032 (AY INOMOTO CO. INC) 7 mars 1984, 'voir revendications 1-8; page 9, 1,3,4,5,6 ligne 24, page 10, ligne page. 'LJgne 23 -page 11, ligne 9; page 13, lignes page .1ignes. exeinpies I, A EP, A, 0109771 (GENERAL FOOD C0OP0RATI0N) mait 1984, voir o.evendi cations 1,4 1-6 A PA, 0106910 (AJINOMOTO CO.) 2 mai 1984, voir revendications 1-5 1-11 A FR, A, 22452,99, (GENERALL FOOD CORPORATION) avril 1975, voir revendlications 1,2; 1-11 exeinpies 1,3 Catkgories sotciates do, documents citoft 'I eT document ultilie'ir pubilit 0poat6rieurementhlisdaddp6t iAiidocument dotinisant Pltat gitnitrai do I* technique, non Inentoa OU A is date do orlorit# at n~sooorionant pas consditit cmme arti~liremet prtinnt II'tat d Istechnique oiortinent, molt citil pout comorendro aIxdcuna i ot co m at a oiuitt A spe a* on t issa 1.Principe ou Is rnoorie constituent Ia bass do l'invenition e Es documentrenpCott*r, datie *ui0h.dt odi~ nen.~~i document Pariiculw~oment oertinontt' i'inventlon revondi. tioni o aprs Ctte atequite no pout Atto considire comms nouvelie ou Comm. 4 L document oouvent eotr un doute suf une tevendicatlon de Impliquant uno activitt inventive ptlorit* ou cie pout diterminer as date do putblicationt d'n Suit* citation ou Pout une ration soOClule (teli* qutndiquilt), a document panticuliroment orlineilt !'invention revon-, diquile no out Arconsiderie COmme Imaliquent Line it0 it document so 0110rant A une divuigation coai#, i Un Usage. A acIlvit invent Ioreu u a e document oat associt a un ott uric exposidn ou touls suie moyonauers eutres'. docume* nts n doa m me nature ,Cello combl., 4 Is w documenit PUblij avant Is data do divot initnalioml, mais aloan saunt iividonle pout Line personne du mltter, A date do pviorili (evonetquto a La document qui 41 Peltalo deo m4'\j fomuie do brevets IV, CIENTIFICATION Dso 4 Isaueito Is recherchte Intotrialonalt a 6A" etvmn aedepfto upiejrpotdorcoc#itrainl fichole~ ~cteet Dt epdto Upiotrgo orcocoibrotni 4 aoQt 1986 Administration chariie do ts recherh Interntional* Sgnaotue du tqnctionntre4 fill...1 OFFCE: iRopE DEs BRE-VETS M. \?AN Formuiast PCTIISA/210 (dousilire loutlle) (Jeate, I111) I'. q I IIIIIIIII0 1fir k V ANNEXE AU A.APPORT DE RECHERCHE INTERNATIONALE RELATIF A LA DEMANDE INTERNATIONALE NO. PCT/FR 86/00158 (SA 13154) La pr~sente annexe indique les membres de la famille de brevets relatifs aux documents brevets cit~s dans le rapport de recherche international vis6 ci-dessus. Lesdits membres sont ceux contenus au fichier informatique de l'Office europ~en des brevets A la date du 13/08/86 Les renseignements fournis sont donn6s A titre indicatif et n' engagent pas la responsabilit6 de 1'Office europ~en des brevets. Document brevet cit6 au rapport de recherche Date de publication Membre(s) de la famille de brevets Date de publication EP-A- 0102032 07/03/84 JP-A- 59031669 20/02/84 JP-A- 59031656 20/02/84 EP-A- 0109771 30/05/84 Aucun EP-A- 0106910 02/05/84 Aucun FR-A- 2245299 25/04/75 Aucun Pour tout renseignement concernant cette 5 anrw .ce voir Journal Officiel de l'Office europ6'rn cdes brevets, No. 12/82