AU675230B2 - Use of stabilized milk-protein powder in the production of process cheese and cheese preparations, and methods of manufacturing such products - Google Patents

Abstract

The invention concerns the use, in the production of process cheese and cheese preparations, of stabilized milk protein, or casein, in the form of a dry powder containing 0.5 to 20 % of phosphate and/or citrate and with a protein content of over 30 % relative to the dry product. The invention also concerns methods of manufacturing such process cheese and cheese preparations.

Description

OPI DATE 31/01/94 AOJP DATE 28'i04/94 APPLN. ID 45674/93 PCT NUMBER PCT/FP93/01813 AU9345674 INTERNATIONALE ZUSAMMENARBEIT AUIF IDkM GEBILiT DES PATEiNTAVESENS (PCT) (51) Internationale Patentklassifikation 51 A23C 19/082, A23J 3/08 L(11) Internationale Ver~irrentlichungsnumrner: WO 94/01000 Al j(43) lnterniitlonales Veriiffentlichungsdatum: 2.0, Januar 1994 (20.01.94) (21) lnternutionales A1ktenzelchen: (22) Intemalionales Anmeldedatum: PCT,'EP93 10I81' 10. Juli 1993 (10.07.93)1 Priorltiltsda ten: P 42 22 .875.1 11. Juli 1992 (11.07.92) (71) Anmelder (Pt r alle lkstimmtungssawn ausser L'S) 13K LA- DENBURG GMBH IDE#DEJ; Dr. Albert. Reimann-str.

2, D).68526 Ladenburg DANMARK PROTEIN A/S IDK'DKI; Nr. Vium, DK-6920 Videbick (DK).

(72) Erfinder; und Erfinder/Anmelder (nur fir US) MERKENICH, Karl jDE'DEJ; Am Rimbacher Weg 13, D-64658 FilrthlFahrenbach MAURER-ROTH MANN, Andrea IDE/ DEJ; Siegfriedstr. 14, D-69469 Weinheimn SCHEU- RER, Gunther IDE/DE); Kirchgasse 61, D-67454 Haglochl WALTER, Edgar (DE/DEJ1; Gerhard-l-auptmann-Str. 28, D-68169 Mannheim ALBERTSEN, Kristian [DK/DKJ; Bogclyvej 16, Skovby, DK.Videbaek WILMSEN, Arnd [DK/DKI; Kildeliojvej Giellerup, DK-7400 Herning (DK).

(74) AvwA211 GRUSSI)ORF. Jurgen. Zellentin Partner, Ruhensstr. 30, D.67061 Ludwigshafen (DE).

(81) Bestimmungsstaaten: AU, CA, Fl, JP. KP, NO, NZ, RU, US, europ~1isches Patent (AT, BE, CH, DE, DK, ES, FR, GBl, GR, IE. IT, LU, MC, NL, PT, SE).

Verblfentlicht Alit internationak,.n Rechcdenberich.

6753 (54)Titlc: USE OF STABILIZED MILK-PROTEIN POWDER IN THE PRODUCTION OF PROCESS CHEESE AND CHEESE PREPARATIONS, AND METHODS OF MANUFACTURING SUCH PRODUCTS (54) Bezeichnung: VERWENDUNG VON STABILISIERTEN MILCHPROTEINPULVERN ZUR HERSTELLUNG VON SCHMELZKASE UND KAiSEZUBEREITUNGEN SOWIE VERFAHREN ZU IHRER HERSTELLUNG (57) Abstract The invention concerns the use, in the production of process cheese and cheese preparations, of stabilized milk protein, or cascin, in the form of a dry powder containing 0.5 to 20 96 of phosphate and/or citrate and with a protein content of over 30 %V relative to the dry product. The invention also concerns -iethods of manufacturing such process cheese and cheese preparations.

(57) Zusammenfassung Die vorliegende Erflndung betrifft die Verwendung von stabilisiertem Molkenprotein oder Casein in Form eines trockenen Pulvers. das 0,5 bis 20 Po Phosphat und/oder Citrat und einen Proteinanteil von Olber 3000o der Trockensubstanz enthialt, zur Herstellung von Schmelzk,1ise und Kilsezubereitungen sowie Verfahren zu ihrer Herstellung

IL.

Use.of stabilised milk protein powder for the production of processed cheese and cheese preparations, as well as processes for their production The present invention concerns the use of stabilised protein powders for the production of processed cheese and cheese preparations, as well as processes for their 2roduction..

Processed cheese preparations were already produced for the first time in the year 1911 and later, with changing composition of the starting materials, continuously improved in flavour, in appearance and in the texture. Depending upon the composition, there can thereby be obtained spreadable or cuttable products.

15 Starting material is ai cuttable cheese, such as Gouda, Emmentaler etc., which is comminuted and mixed and melted at temperatures of about 80 to 95 0 C together Swith fat, especially butter, and processing salts, as well as possibly some water, whereafter the mass is 20 shaped, cooled and packed.. As processing salts, there are used trisodium citrate or sodium phosphate or their mixtures, mostly in the form of commercially available hydrates. Furthermore, processed cheese frequently also contain binding gents or thickeners, for example starch, guar flour, pectin, carboxymethylcellulose, agar agar, alginates or similar products. Instead of the expensive hard cheeses, there can also be used, to a small extent, cheese substitute materials, such as 2 casein, whey powder, curds, yoghurt, milk protein, and, to a certain extent, also vegetable proteins, especially soya protein. In this connect?-n, the use of natural milk proteins, such as they occur in whey powder and casein, would be especially interesting.

However, it is known that these may be added to the processed cheese only in small amounts whey powder up to about casein up to about 10%, rennet casein up to of the processed cheese mass since, in the case of larger amounts, these proteins crystallise out from the processed cheese mass and thus impart a "sandy consistency" to the processed cheese or become visible as Etrippling or even impart a bitter taste to the whole mass. (Die Schmelzkdseherstellung, Johaleitfaden, Benckiser Knapsack, 1989, pages 93-96).

Therefore, there exists a need to change whey proteins or casein, so that they can be added to a :processed cheese preparation in amounts of 10 to 20% by weight of the processed cheese without precipitating out or 20 changing the taste of the product.

We have surprisingly found that this task is attainable by the features set out in the main claims and Sis enhanced by the features set out in the subsidiary S. claims.

S 25 According to DE-AS 25 22 508, a suspension of casein which contains not more than 270 g casein/l is first ripened with citric acid or phosphoric acid at pH values of "not under Subsequently, by addition of alkali, the pH value is again lowered to staWaeldraftsl45674.93_3 10.1 3 6.8 to 7.5, respectively. The so-obtained products can be concentrated or dried by some process and thereby give a caseinate which can be directly dissolved in water, whereby a true solution or a colloidal solution of a gel is obtained. The usability of such products in cheese preparations, in which it is a question of the emulsifiability of the proteins, is not described.

In EP 0 076 685 is described a process for the production of whey proteins which display an improved gel formation, whereby the pH value of the whey protein solution is first to be increased to 8.5 11.5 in order to increase the "sulphhydryl group count", whereafter to the solution are first added comparatively weak 15 acids, such as citric acid, phosphoric acid or polyphosphoric acid, and subsequently a strong acid, such as hydrochloric acid or sulphuric acid, in order to adjust the pH of the solution to 6 to 8. Due to the depolymerisation of the sulphhydryl groups in alkaline solution, the water solubility is, on the one hand, improved and, due to recombination of sulphhydryl bridges, on the other hand, the gel formation is brought about. A use of such products as additives in processed cheese is not to be deduced from this document.

From Journal of Food Science, 1984, No. 1, pages 32, 33 and 39 is known again to dissolve whey powder (WPC whey protein concentrates) in water for the 4 further working up in that one adds a sodium orthophosphate in an amount of 0.1 0.25% w/w of dry protein powder and tempers the solution to 75 85 0 °C before a heat sterilisation is carried out. For the resolubilisation, it is possible but less favourable to add the phosphate as in the case of the production of the whey powder.

Surprisingly, however, such products are very well suited for the production of processed cheese, whereas the subsequent addition of phosphates to once dried WPC proved to be useless.

The proteins used according to this invention can be added to a processed cheese preparation in amounts of up to 20%, by weight of the processed cheese. This wide range of whey protein can replace the casein previously added in amounts of about 5 to 10% of the cheese mass, and achieve the necessary hardness of the cheese preparations. The native whey protein powder stabilised with phosphates or citrates can dissolve surprisingly easily in the cheese mass and do not tend to crystallise so that the finished, processed cheese display neither a sandy texture nor external stipples, even after comparatively long storage.

The term "Native Whey" means whey that is not chemically processed or dehydrated prior to use.

It is assumed that this stabilisation is due to the fact that phosphate or citrate molecules become incorporated, under the conditions used in accordance with the invention, into the tertiary structure of the protein so that it is stabilised in the subsequent drying. Thus, the protein must obviously be treated in solution with these compounds since once precipitated out and dried the protein cannot be converted by resuspending in water and treating with phosphates or citrates to turn it into the corresponding structure conducive for a mixing with processed cheese, unless a very long period of time has elapsed before re-suspension is undertaken. A mixing of whey protein, in unstabilised form, with sodium phosphates staftlakeep/Speci 45674.93 5996 4a or citrates even in substantially higher concentrations in which they are used as processing salts (1.5 to 3% by V stat1JakoepSpea.45674.93 5,.96 5 weight of the dry whey protein) does not lead as said above to a stabilised product. Thus, these should only be added in small amounts.

For the production of the stabilised whey powder of the present invention, one preferably starts from the whey obtained in large amounts in the production of curds and cheese and which is concentrated by ultrafiltration or other known processes and, at the same time, is freed from a part of lactose and salts contained. An average whey may therefore contain, by weight, about 0.9% protein, 0.1% fat, lactose and 0.7 g inorganic salts. Such a whey is concentrated, for example, to 30% dry weight, whereby the concentrate contains, for example, 16% protein (56% in the dry weight), 1.6% fat in the dry weight), lactose (33% in the dry weight) and 1.4% inorganic salts in the dry weight). To this concentrate are added 0.2 0 to 5% (by weight of a solution of the dry concentrate) of a e processing salt of the group ortho-, di-, pyro- and 0: polyphosphate (together designated as phosphate) and oo* 20 citrate, whereby the sodium salts are preferred but potassium or ammonium salts may also be used. The addition should amount to about 0.5 to 20% of the dry weight ;of the whey protein concentrate. A concentration of 1 to 5% (w/w of dry weight) are the optimum values for achieving stabilisation. Amounts above 20% w/w dry weight are uneconomic since the processing salt concentration necessary for the production of the processed cheese is thereby also exceeded. A concentration of below 0.2% of the solution or below 0.5% w/w of the whey protein concentrate used does not bring about a sufficient stabilisation so that these products do not differ from known whey protein powders. The addition of the stabilisers preferably takes place as a 1 to 10% solution in water and it is, however, also possible to add higher concentrations, for example 10 to 50%, as a slurry in order to avoid diluting the protein solution unnecessarily. An slafilaelkeeplspecV45674.93_3 18.1,96 6 addition as dry powder is admittedly possible but, because of poor miscibility, this is not preferred.

The whey protein to be stabilised in accordance with the invention may be sweet or acidic whey adjusted by ultrafiltration, with partial removal of water, lactose and dissolved salts to a protein content of 3 to 30% in the solution, the protein content in the dry mass being 30 to 96% by weight, before addition of phosphate and/or citrate.

The addition of the processing salts as stabilising agent takes place in a pH range between 2.8 and preferably in the pH range of about 7.0 to 4.0, in which the protein solutions in question are stable.

In order to accelerate the equilibrium adjustment between phosphate and protein, it has proved to be 15 advantageous to warm the solutions, to temperatures of to 150 0 C, preferably 50 to 90 0 C, and, depending upon the temperature, reaction times of 2 sec. to about 10 min, are necessary. In the case of temperatures above the boiling point, one must naturally work with a corresponding, higher pressure. The warming can take place by means of appropriate heat exchangers, such as plate heat exchangers, tube heaters, chafing heaters or by direct or indirect heating with steam.

The drying of the protein solution which is stabilised according to the inventicn to form the stable, end product takes place in the usual way with spray driers, spray towers, fluidised bed driers but also with roller driers and other known apparatus. The moisture content of the end product should lie below preferably 2 of the dry product.

By means of the joint spraying of the whey with processing salts, especially phosphates, it is possible to improve the functional properties of these proteins. These functionally changed proteins can be used in processed cheese, processed cheese preparations, fresh cheese and fresh cheese preparations of processed cheese, imitation staff/aikeep/Spec 45674 93 59.96 7 cheese, reconstitutions, pizza toppings, bread spreads, cheese dips and cheese sauces, whereby adding 5 to whey protein (WPC) to the dry product do not change consistency, appearance and taste of the finished product.

In the case where smaller amounts of the stabilised proteins according to the inveriion or in the case where a smaller amount of processing salt are used to stabilise the protein, it may be necessary to incorporate additional amounts of processing salt into the cheese mixture in the usual way. The other components of these processed cheese compositions according to the in\mntion correspond to that which is analogously known for such products.

The following flow scheme, which contemplates unstabilised whey proteins of differing concentration and 15 composition, gives the best mode of carrying out the process according to the invention.

V.

20 .o a :1 20 oooo o* dry weight W/W) protein in dry product name of Whey Concentrate weight of whey concentrate W/W) 15 50 33 3 15 50 55 3 15 50 65 3 15 50 77 3 15 50 84 2 WPC-76 40 91 2 WPC-83 40 96 2 WPC-88 1. All WPC types (whey protein concentrate) can be produced not only with sweet but also with acidic whey.

In the cases of use of these whey types, one obtains a WPC between pH 2.8 and 2. Added amount of the phosphates or citrates or mixtures of phosphates and citrates is: 0.5 to preferably 1.0 to calculated on the dry weight of the whey protein concentrate solution; addition is to 1 to solution or 10 to 50% slurry of WPC.

staff/alkeeplSpeci.45674.93 5.9.96 8 3. pH range for the pH adjustment step is 2.8 to 4. Temperature treatment in a T-range between 35 co 150 0 C, period of time: 1 sec to 10 min.

5. Heat transmission: plate heat exchanger, tube heater, chafe heater, direct or indirect UHT process.

6. Spray drying: spray tower; nozzle or rotation spraying; e.g. niro atomiser, swirl fluidised, roller drying, belt dried; e.g. filter mat type.

4 4.

Description of the production process protein solution 1. 100 kg (30 kg in dry weight) protein 54.3% in dry wt.

phosphate mixing 3 -150C 2.

3.36 kg 25% H 2 0 pH adjustment pH temperature treatment spray drying 3. Na-, Ca-OH solution 4. 72 0 C/15 sec.

cooling to 55 0

C

plate heat exchanger 6. inlet temp: 180 0

C

outlet temp: 75 0

C

end product 35.5 kg powder 52.7% protein in dry wt.

The use of the stabilised whey protein according to the invention fur the production of processed cheese preparations is hereby examplified to explain the invention slafWalkeep'Spea 45674 93 6 9 96 9 but the examples do not limit the invention. As one can see from the examples, a stabilisation of the whey proteins brings about a substantial improvement of the appearance and of the consistency of the cheese obtained. Protein proportion in the whey proteins of below 30% in the dry substance or an insufficient phosphate stabilisation (native proteins) proves to be not usable.

Example 1 Spreadable processed cheese preparation (49% dry wt. 61% fat in dry Addition of 5% stabilised whey protein (96% w/w protein in dry substance) in end product:- Basic rezipe 750.0 g Cheddar (50% fat in dry wt.) 750.0 g Gouda (50% fat in dry wt.) 521.7 g butter (84% fat in dry wt.) 75.0 g whey protein (96% w/w protein) in dry substance 47.3 g JOHA S 9 (JOHA is a registered trade mark of BK Ladenberg GmbH) 815.2 g water inc. condensate Heating of the additives within 9 min to 90 to 92 0 C, direct steam introduction; stirring speed 120 r.p.m.

Variants (for 5% w/w WP 96% w/w protein in dry substance) of the above-mentioned basic recipe: 25 a. native whey protein with a protein content of 80% w/w of the dry whey.

sensory assessment: appearance outer: sticks to the foil inner: coarse consistency: to, solid, atypical taste: not marked b. native whey protein, protein content 60% of dry whey.

staffl/a epfSpeci.4567493 5.9.96 9a sensory assessment: appearance outer: inner: consistency: taste: sticks to the foil coarse too solid, atypical not marked 9 9 9 9*9* 9S 9* 9* ~9

S.

9 9 9S** PWL&op;Sp 45%7493 59 9G 10 c. native whey protein, protein content 35% of dry whey.

sensory assessment: appearance outer: sticks to the foil inner: coarse consistency: too solid, atypical taste: not marked d. whey protein modified with JOHA SDS 2, protein content of dry, modified substance.

sensory assessment: appearance outer: sticks slightly to the foil inner: in order consistency: creamy taste: typical 15 e. whey protein modified with JOHA S 9, protein content of dry, modified substance.

sensory assessment: o appearance outer: sticks slightly to the foil inner: in order S: 20 consistency: creamy taste: typical f. whey protein modified with JOHA SDS 2, protein content of dry, modified substance.

sensory assessment: 25 appearance outer: sticks slightly to the foil inner: in order consistency: creamy taste: typical g. whey protein modified with JOHA S 9, protein content of dry, modified substance.

sensory assessment: appearance outer: sticks slightly to the foil inner: in order consistency: creamy taste: typical h. whey protein modified with JOHA SDS 2, protein content taWaeakeospecVW4574.93_3 18.1.96 11

S

S

9 of dry, modified substance.

sensory assessment: appearance outer: sticks to the foil inner: slightly coarse consistency: atypical, coarse taste: not marked i. whey protein modified with JPHA S 9, protein content 30% dry, modified substance.

sensory assessment: appearance outer: sticks to the foil inner: slightly coarse consistency: atypical, coarse taste: not relevant The whey containing 60% and 80% (w/w dry 15 substance) protein and modified with JOHA SDS 2 and with JOHA S 9 show in the end product a loose, shiny and creamy consistency. However, modified proteins from 30% of dry whey are also still usable.

The non-modified whey proteins, as well as 20 modified whey proteins with protein contents below of dry whey do not show the desired results. The consistency of these processed cheeses is too solid, coarse, the surface is dull, one sees stipples.

For the modification of the whey proteins with phosphates, with JOHA SDS 2 was chosen a phosphate combination with highest possible orthophosphats part, with JOHA S 9 was used a phosphate mixture with highest possible polyphosphate part.

Example 2 Production of block processed cheese (54% dry wt.

48% in the dry wt.) staWaeahkcGspGcV45674.93_ 18.1.96 12 Replacement of rennet casein by modified whey protein:basic recipe (comparison): (invention) 1000.0 g Chester (50% FiD) ditto 250.0 g Gouda (50% w/w FiD) ditto 250.0 g Viereck hard cheese (45% w/w ditto FiD) 80.0 g butter (94% w/w of dry ditto product) 15.0 g JOHA PZ 7 ditto g JOHA T ditto 80.0 g rennet casein 80.0 g whey protein (protein content about 73% w/w dry whey) (phosphate content 3% w/w of whey protein) Melting period 10 min., 120 melt temperature 70 to 75 0 C; 350.0 g water, inc. condensate (addition 200 g) (FiD fat in dry weight) Assessment of the remeltability: invention with WP comparison rennet casein a. rubbability slightly sticky in order grillability after 5 days: good nil after 20 days: good slight toastability after 5 days: in order in order after 20 days: toast value 4 toast value 6 fat loss after 5 days: excellent no after 20 days: little scarcely threadiness stafflae/drafts/45674.93_3 10.1 13 o

J

o after 5 days: no no after 20 days: slight slight Production of modified whey proteins 1. Modification with JOHA SDS, JOHA S 9 Protein contents 30 to 80% of dry whey.

Analysis:.

WP 80% A L A 2 total P20 5 0.96 2,29 2,47 P-chrom. mono mono, start mono, start protein 75.61 76,94 77.64 ash 2..34 4.33 4.58 pH (10) 6.4 solubility 96% 98% A 1 and A 2 modified whey proteins WP 80 non-modified whey protein concentrate Addition of a 25 to 30% slurry, referred to the retentate 1% JOHA S 9 or 1% JOHA SDS 2, mspectively.

(JOHA is a Registered Trade Mark of the Applicant).

stafflae/drafts/45674.93_3 10,1 -14 Example 2 Acidic whey 2000 kg with a content of 0.9 protein, 0.1 fat, 4.5 lactose, 0.7 g inorganic salt and a pH of about 6.0 is ultrafiltrated through cellulose membrane to give 10 kg of a retenate concentrate which contains 18 protein, 1.6 fat, 9.5 lactose and 1.4 inorganic salts.

0.82 kg of a mixture of 90 sodium orthophosphate and 10 sodiumpolyphosphate in 10 kg water is added at 10 0 C and the pH adjusted to 6.5 by addition of a 0.1 M sodiumhydroxide solution. Then, the mixture is heated to 72 0 C for 15 seconds and re-cooled to 55 0

C

thereafter. This product is spray dried in a spray tower with an air inlet temperature of about 180 0 C and an outlet 15 temperature of 75 0 C to 35.5 kg of a dry powder of modified whey with a content of 52.7 protein, 5.3 fat, 31.3 lactose, 7.3 salts and 3.4 residual water.

o* *l o stathfrorkeeplspela457493.BKLANDNBERG 25.11

Claims (9)

1. A method of producing processed cheese, comprising the step of adding a maximum of 20% (w/w of said cheese) of stabilised whey protein powder to cheese; said stabilised whey protein being produced by: i) mixing protein enriched native whey concentrate with 0.5 to 20% (w/w of said whey) phosphate and/or citrate salt at a pH of between 2.8 to 8.0, said phosphate being selected from the group consisting of ortho-,di-,pyro- and poly-phosphate and said salt is selected from the group consisting of sodium, potassium and ammonium salt, (ii) heating the mixture of step to a temperature of 35-150 0 C and (iii) drying the mixture from step whereby the whey protein comprises over 30% of the dry weight of the stabilised whey. A method according to claim 1 wherein the heating in step (ii) is at a temperature of 50 to 100 0 C. 20 3. A method according to claims 1 or 2 wherein the amount of stabilised whey protein powder added to the cheese is 5 to 10% of said cheese.

4. A method according to any one of claims 1 to 3, wherein, in step i) 1 to 5% (w/w of said whey' phosphate or citrate is used. A method according to any one of claims 1 to 4, wherein the whey protein comprises 50 to 96% of the dry weight of the stabilised whey.

6. A method according to any one of claims 1 to wherein the whey concentrate contains 0 60% (w/w of dry concentrate) lactose and 0 to 10% (w/w of dry concentrate) of inorganic and organic salts.

7. A method according to any one of claims 1 to 6, wherein the stabilised whey protein powder still contains 2 to 7% (w/w of dry powder) of water. staffa/keeplSpeci45674 93 69 96 *t

8. A method according to any one of claims 1 to 7, wherein the whey protein powder to be stabilised is sweet or acidic whey which is adjusted by ultrafiltration, with partial removal of water, lactose and dissolved salts to a protein content of 3 to 30% in the solution and the protain content in the dry mass is 30 to 96%, before the phosphate or citrate is added thereto.

9. A method according to any one of claims 1 to 8, further comprising the step of adding fat, processing salts, water and other usual components, melting the resulting mixture, forming a melt mass and cooling said mass.

10. A method according to claim 9 wherein the stabilised whey protein powder added to the cheeses is 15 20% (w/w of processed cheese).

11. A method according to any one of the preceding claims, with reference to the examples. DATED THIS 6th DAY OF September 1996. B K LADENBURG GMBH DANMARK PROTEIN A/S 20 By its Patent Attorneys: GRIFFITH HACK Fellows Institute of Patent Attorneys of Australia sta alkeeplSpoe.45674.93 6.9.96 INTERNATIONAL SEARCIl IMPOR' International application No. PCr/EP 93/01813 A. CLASSIFICATION OF SUBJECT MATTER INT. CL. 5 A23C19/082; A23J3/08 According to International Patent Classification (IPC) or to both national classification and IPC B. FIELDS SEARCHED Minimum documentation searched (classification system followed by classification symbols) INT. CL. 5 A23C A23J Documentation searched other than minimum documentation to the extent that such documents are included in the fields searched Electronic data base consulted during the international search (name of data base and, where practicable, search terms used) C. DOCUMENTS CONSIDERED TO BE RELEVANT Category* Citation of document, with indication, where appropriate, of the relevant passages Relevant to claim No. X DE, A, 2 342 299 (CHEMISCHE FABRIK BUDENHEIM 1, 3, 4, R.A. OETKER) April 1975 see page 4, paragraph 2 paragraph 3; claims 1, 2; example X US, A, 4 166 142 CHANG) 1, 2, 28 August 1979 see column 1, line 66 column 2, line 31; claim 1 X JOURNAL OF FOOD SCIENCE 6, 7 Vol. 49, No. 1, 1984, CHICAGO US, pages 32-33 39 I. BARLOW ET AL. 'Stability of reconstituted whey protein concentrates to ultra-heat-treatment processing' see page 32, column 1 page 33, column 1; table 3 S Further documents are listed in the continuation of Box C. See patent family annex. S Special categories of cited documents: laterdocumentpublishedaftertheinternational ilingdateorpriority document defining the general state of the art which is not considered date and not in conflict with the applcation but cited to unerstand to be of particular relevance the principle or theory underlying the invention earlier document but published on or after the international filing date document of particular relevance: the claimed invention cannot be considered novel or cannot be considered to involve an inventive document which may throw dotbts on priority claim(s) or which is step whe n the documennt is taken aloneee e e cited to establish the publication date of another citation or other ste w he docume s ak al special reason (as specified) document of particular relevanoc; the claimed invention cannot be document referring to an oral disclosure, use, exhibition or other considered to involve an inventive step when the document is means combined with one or more other such documents, such combination document published prior to the international filing date but later than being obvious to a person skilled in the art the priority date claimed document member of the same patent family Date of the actual completion of the international search Date of mailing of the international search report 29 September 1993 (29.09.93) 07 October 1993 (07.10.93) Name and mailing address of the ISA/ Authorized officer EUROPEAN PATENT OFFICE Facsimile No. Telephone No. Form PCT/1SA/210 (second sheet) (July 1992) INTERNATIONAL SEARCH REPORT Internaional application No PCT/EP 93/01813 C (Continuation i. DOCUMENTS CONSIDERED TO BE RELEVANT Category' Citation of document. with indication, where appropriate. of the relevant passges Relevant 1o claim No. A DATABASE WPI8 Section Chi. Week 7108 Deriwent Publications Ltd., London, GB; Class D13, AN 71-14814S JP', B 46 006 813 (WAKODO CO) 1971 see abstract A H. KLOSTERMEYER 'Die Schmelzkiiseherstellung' 1989 BEN KI SER KNAPSACK, LADEN'BURG, DE see page 93 page 96 Fc~rm PCTISA/210 tcontinuauon oi secona shezt) (July 1992) ANNEX TO THE INTERNATIONAL SEARCH REPORT ON INTERNATIONAL PATENT APPLICATION NO. EP 9301813 SA 76752 This annex lists the patent family members rclating to the patent documents cited in the above-mentioned international search report. The members are as contained in the European Patent Office EDP flc on The European Patent Office is in no way liable for these particulars which are merely given for the purpose of information. 29/09/93 Patent document Publication Patent family Publication cited in search report I date member(s) Idat e OE-A-2342299 10-04-75 None US-A-4166142 28-08-79 AU-A- BE-A- CA-A- CH-A- DE-A- FR-A, B GB-A- JP-A- ~JP-B- NL-A- SE-B- SE-A- 8793475 838139 1090195 618585 2603416 2298956 1525791 51101165 59018022 7600447 428340 7601083 07-07-77

30-07-76 25-11-80 15-08-80 05-08-76 27-08-76 20-09-78 07-09-76 25-04-84 05-08-76 27-06-83 04-08-76 01 0 M For more details abluut this annex see Official Journal of the Europewi Patent Office, No. 12/82 I NTERNATIONALER RECHlEIRCI EN BERICIHr Interiationales Alitcnzelchen PCT/EP 93/01813 1. KLASSIFIKATION DES ANNIEIDUNGSGEGENSTANDS (bel mebreme Klassiftkatdonssymboien sid a le augeben)6 Nach der internationalen Patcatklassirikation oder nah der nationalen Klassifiuiation und der IPC Int.Kl. 5 A23C19/082; A23J3/08 UI. RECHERCIUERTE SACHGEBIETE Recbechdleiter Mindestprilfstaff 7 Rechercbierte nicht zurn bindestpriffstoff gebbrende Vctiffeatllcliungen, soweit tiese unter die re dlerten Sachgebiete fallen 3 ill. EINSCHLAGIGE VEROFFENTUCI{UNGEN~ Art. jenzjchnni der Vr*Jffentlidiungl soei erodec unter Ang-abe der mallgeblchen Telle 1 Reai. Ansprucli Nr. 1 3 X DE,A,2 342 299 (CHEMISCHE FABRIK BUDENHEIM 1,3,4,5 R.A. OETKER) April 1975 siehe Seite 4, Absatz 2 -Absatz 3; AnsprUche 1,2; Beispiel X US,A,4 166 142 CHANG) 1,2,5 28. August 1979 siehe Spalte 1, Zeile 66 -Spalte 2, Zeile 31; Anspruch 1 0 Bcsondere Kategorien von angegebenen Vrilffeticungn 1 0 Verilffeatlichung, de den allgm ec Stund der Tedinik Splstetc Vcr~wlcatlichundeasidmittntolnA- definicit, abet tuicbt Lis besogas bedeutsam an-schea ist meldedatu den Voritltsdiaturn veroifentlicit worden Mteres Dokument, das jedoch eist am oder nad dem interns- ist unt' der Anaselduag, niclit kollidiert, snndai alit zam tinlnAnmeldedaturn vediffentliebi worden 1st Verstlindlals des der Erfindang zugrunddiegenden Priazips tionlenoder der ibi wgrundeiiegcnden Tbeorie angrgeben 1st Verdffentlicbung, die pseigact 1st, elata Pdioritltsansprudi 'X Veitlffentlidiang voa besondeai Bedeutung, die beanspiucb- zweifelbaft erscheinea an [amen, oder dumbh die djma Verbf-teEfnngknndims caetsfefldudi Tt- fcntlichungsdatum einet anderen im, Redcedienbodcht go-.eEfnugkn ih l euoe u ridrshrTtg aanten Veroffentlichung belegt werden soil oder die aus eine keit betubend betraditet werden anderen besoaderen Grand anlpegeben ist (wie asgefuhut) 'Y Vertiffentlidiuag van besondcee Bedeutung;, die bemnpruch- ''Vcriffeatichung, die sick, auf .me astindlie Offenbatng te Erfinduag kann nidit Ws ant etflnderiscbci Titigkeit be- ruhend betrachtet werden, weun die Ver~ffcntlidiung mit eine Beautxun&, tine Aussteliaag odet andere Maflnahmen eaine oder menremn andsen Veriftlficbuagen dieser Kate- bezicht gone In Verbindung gebracht wttd and dies. Vebiladung flit 'P Verbientlichung, die var dem iaternationalen Anmeddeda- einen Fachmann nabeliegend 1st turn, abet nach dem beansprucbten Priarit!stsdatum veidffent- W Verliffntlichang, die Mltglled derseiben Patentfamilie ist lit warden Ms IV. 8ESCIIEINIGUNG Datum des Abschlusses der inteinatdonalen Recherche Absendediatumt des Intemntlonalen Rsdicidenbalchts 29.SEPTEMBER 1993 07. 10. 93 Internationale Rechbeenbehirde Untetsditift des btvolimitigten Bediensteten EUROPAISCHES PATENTAMT DESMEOT G .R .A. ParubliI PCTIMSA1lI (BlA2tS) tJe-= 19U) INTIERNATIONALEMRELCIIERCJIENBIERICII'I'/P93011 Inteationales jjktenzelcen~i P TE 3011 Ii. EINSCIILAGIGE VEROFFENTUCHIJNGEN (Fortsewing van Blatt 2) Art Kennzelctinung der Veraffentfichung, soweit cifordeflich tinter Angabe der mallgebllihe Telle Bevr. Anspruci Nr. X JOURNAL OF FOOD SCIENCE 6,7 Bd. 49, Nr. 1, 1984, CHICAGO US Seiten 32-33 39 I. BARLOW ET AL. 'Stability of reconstituted whey protein concentrates to ultra-heat-treatment processing' siehe Seite 32, Spalte 1 -Seite 33, Spalte 1; Tabelle3 A DATABASE WPI 8 Section Ch, Week 7108, Derwent Publications Ltd., London, GB; Clasb D13, AN 71-14814S JP,B,46 006 813 (WAKODO CO) 1971 siehe Zusammenfassung A H. KLOSTERMEYER 'Die1 Schmelzkdseherstel lung' I89 BENCKISER KNAPSACK LADENBURG, DE siehe Seite 93 Seite 96 1.Mm~iit PCTr/Is~O (ZmazJmee) (Jinwr 1945) I i ANHANG ZUM INTERNATIONALEN RECHERCHnNBERIC'iT OYBER DIE INTERNATIONALE PATENTANMELDUNG NR. 9301813 76752 In diesem Anbang sind die Mitgfiedtt der Patentfamilien der ii obengwnannten internstionalen Rech cheeicht angefihrten Patentdokumente angegeben. Die Angaben iiber die Familieixmitgfieder entsprchien deni Stand der Datei des Europuiischen PaLntaznts am Diese Angaben dienen nur zur Unterrichtung und erfolgen ohne GcwiLhr. 29/09/93 Im Recherdienher~ht k~atum icr Nlitglied(er) der angefillrtes Patentdokunment DE-A-2342299 Ver~ffatidug 10-04-75 Patmdtamwli K(eine flktum cder Ve~efji!m US-A-4166 142 28-08-79 AU-A- 8793475 07-07-77 19 BE-A- 838139 30-07-76 CA-A- 1090195 25-11-80 CH-A- 618585 15-08-80 DE-A- 2603416 05-08-76 FR-A,u 2298956 27-08-76 GB-A- 1525791 20-09-78 JP-A- 51101165 07-09-76 JP-B- 590018022 25-04-84 NL-A- 7600447 05-08-~76 SE-B- 428340 27-06-83 SE-A- 7601083 04-08-76 4-i Fur nihemt Einzeiheitct. 4iesem Anhang :siebe Amtisbatt des Europiischen PatecWtmt Nr.12IB2