DE2649406A1 - Fruit pectin deriv. prepn. - from low esterified pectin mixt. with phosphate in aq. acid soln. by addn. of metal salt - Google Patents

Abstract

A fruit pectin deriv., esp of apple pectin, for making jellies having a partic. low dry solids content, is prepd. by using a pectin raw material having a metal bonding capacity of 30-140 g. metal salt, calculated as CaCl2, for each kg. pectin at degree of esterification 30-40 (35-38)%. A soln. having pH 4.4-4.8 is prepd. from the pectin raw material, water and phosphate, at 10-90 degrees C. A determined metal salt quantity is added to the sln. and the pectin deriv. formed is pptd. from the soln. and dried. The phosphated Ca pectinate obtd. is soluble in cold and warm water, and forms a soln. having low viscosity, which allows easy working. The Ca-phosphate Cpd dissociates at a given pH in cooking, to form the original low esterified pectin in a defined Ca- and buffer concn. A uniform Ca pectinate gel is formed. The pectin deriv. is similar to amidised pectin as regards Ca- and pH-dependence.

Description

Process for the production of a pectin derivative on the

Basis of fruit pectin - ====== The invention relates to a method for the production of a pectin derivative based on fruit pectin, in particular Apple pectin, suitable for the production of jellies with a particularly low dry matter content.

High methylester pectins form gels, with gel formation on a Dehydration and electrical neutralization of colloidally dispersed and hydrated ones Pectin agglomerates. This requires sugar or a sugar substitute as a dehydrating agent be present at a concentration close to 65% and must be the required one pH value must be maintained within a narrow tolerance range. The individual pectin molecules are linked by hydrogen bonds that are given by the sugar.

Low methylester pectins, i.e. pectins with one degree of esterification below 50%, have gelling and thickening properties that are similar to those of agar or are similar to gelatine. Low-esterified pectins are used in the food industry for example for the production of low-dry matter jellies, milk puddings and sugar-free ones Jellies used. The jelly eggs hang from low methylester pek-tins on the amount of pectin, the dry matter, the pH value and the content of buffer salt and the calcium optimum, expressed in concentration, plays a role here not insignificant role, the optimal one depending on the degree of esterification Changes in the amount of calcium ions. The calcium optimum, expressed in mg Ca / g pectin, the forms a firm gel is a defined parameter for a certain pectin. A crossing the Ca concentration results in a brittle gel with a strong tendency to syneresis. The dependence on the pH value and the amount of dry matter only plays a role a subordinate role. For the technological application of these pectins are however, the following factors are unfavorable: 1. The lower the degree of esterification of a pectin the worse is its solubility in water; 2. to maintain an optimal Calcium ion concentration, an addition of Ca is usually necessary, which depends on the water used and the fruit.

The invention has for its object to provide a pectin derivative on the Base of low methylester pectin with the optimum for its degree of esterification Produce the amount of calcium in such a way that at the same time there is a sufficient amount of buffer salt is present to keep this pectin in aqueous solution.

Calcium stands for other comparable substances such as magnesium or the like.

To achieve this object, the process according to the invention is characterized in that a) a pectin is used as the starting material, which has a metal bond calculated as 30 - 140 g calcium chloride per kilogram of pectin with a degree of esterification of 30 - preferably 35 - 38 h, b) produces such a solution from this pectin, water and phosphate that a pH between 4.4 and 4.8 is obtained, c) adding a certain amount of metal salt to the solution, and d) the pectin derivative formed precipitates out of the solution and dries.

Where an advantageous further development of the invention is used The starting material is pectin, which has a calcium binding capacity of 30 - 140 g CaCl2 per kg of pectin with a degree of esterification of 30 - 4050, preferably 35 - 33C; J, whereby in the above-mentioned stage c) a CaCl2 concentration in the form of a solution while stirring vigorously the solution is added.

The phosphate used is in particular polyphosphates, pyrophosphates, especially tetrasodium pyrophosphate.

When using the method according to the invention, a Pectin derivative by reaction of low methylester pectin with certain phosphates produce under the given reaction conditions and given pH. The groomed Pectin-phosphate compound is made to react with calcium ions, whereby one after precipitation a phosphatized calcium pectinate is obtained. From this phosphated Ca pectinate can be assumed that the vast majority of the calcium is not directly bound to pectin but linked to pectin via the phosphate group.

In the technical application, the following is shown Calcium phospho-pectin has the following beneficial properties: Solubility in cold and warm water is good; a relatively low-viscosity solution is formed which a good job guaranteed. When hiring a specific pH value in the boil, the calcium phosphate group is split off Pectin. The original low methylester pectin, which then present in a defined calcium and buffer concentration. The iteaction The pectin with the calcium takes place slowly and a glow-like form is formed Calcium pectinate Gek. Although the dependency on the pH value remains, kaun however, the pH range can be much coarser than with high methylester pectins. the Calcium sensitivity, i.e. the dependence on the fruit or the surrounding area Medium is low. This is according to the invention with regard to the calcium and pH value dependency produced pectin derivative similar to amidated pectin, but with the invention Calcium phospho-pectin the optimal amount of calcium is already integrated.

The method according to the invention is illustrated below using an example explained in more detail: A low methylester pectin with a Degree of esterification of 30-40%, in particular 35-38%, is used.

Determination of the calcium dosage: To determine the necessary Calcium chloride needs cookings with increasing amounts of calcium chloride manufactured. The following recipe serves as a basic cooking (example): 500 g strawberry pulp 500 g low methylester pectin solution 2.5% (= 12.5 pectin) 650 g fructose syrup, 70% approx. 3 ml 50% citric acid to adjust the pH to 2.9.

By stinging to a dry matter content of 50% one obtains a 1 kg cooking.

For every 100 g sample of this boil there are increasing amounts of 2% CaCl2 solution added. The calcium chloride solution is in the still very hot boiling stirred in immediately after pouring out. These samples are used for gelation put aside.

Usually an addition of approx. 2 - 7 ml CaCl2 solution is sufficient. A 2% solution of anhydrous CaCl2 is used. As a measure of the necessary CaCl2 amount serves the consistency of the cooking in such a way that with increasing Strength the best gel strength directly in front of the sample, which starts to become coarse (calcium pectinate formation) is used for the calculation. This corresponds to an addition of 1 ml of CaCl2 solution (2%) to 100 g of the boil with 1.2% low methylester Pectin of a later dosage of 16.67 g CaCl2- (anhydrous) / kg pectin. At a Calcium dosage of 6 ml to 100 g of the boiling corresponds, for example, to a later one Weighing in 100 g CaCl2 per 1 kg low methylester pectin.

As an example, a 30 kg pectin batch was used: a container is filled with 1,200 l of water at a temperature of 50 - 600 C. in the Water are 30 kg of the above-defined while stirring with a high-speed mixer Initial specimen weighed. Then 16.0 kg of tetrasodium pyrophosphate decahydrate are added (Na4P2O7. 10 H2O) was added in solid form to bring the solution to a pH of im substantial 4.4 - 4.8 to be obtained. After adding the pyrophosphate, it takes about 15 minutes stirred for a long time with reduced stirring speed until the pectin is completely has solved.

A higher dosage of sodium pyrophosphate should be used at this time do not take place, de reactions can occur that have an undesirable effect can have on the final quality.

Alternatively, there is the option of using the water first the sodium pyrophosphate and only then the pectin or both fabrics put together.

Then the calculated amount of CaCl is food grade with a degree of purity of about in the form of a 10% solution, preferably about one Injector added with rapid stirring. intensive stirring is necessary, to achieve a quick and good CaCl2 distribution. After adding the CaC12 must be stirred for a while (about 5 minutes) with a high-speed mixer, to ensure an optimal response.

The CaCl2 should be added in such a way that pectinate formation is avoided will.

Instead of calcium chloride, other soluble calcium salts can also be used andjor magnesium salts or mixtures thereof are added; overall can Other salts of polyvalent metal ions can also be added, which affect the food conditions correspond.

A further amount of pyrophosphate is then added.

This amount is determined by taking a sample in the laboratory checks their pH and viscosity. The pH should be set to 5.0 + 0.2 will. A better criterion is the viscosity; Viscosities between 30 - 35 cP at 200 C (measured at 2770 s 1) are acceptable, higher viscosities should not be accepted. The viscosity measurements were made on a Rotovisco at n = 512 rpm with decreasing rotational frequency, 100 S calibration with measuring device NV performed. During this addition of the pyrophosphate present in solid form the high-speed stirrer is used again.

After the zein solution has taken place, this amount of pyrophosphate is used in the laboratory Check the pH and viscosity of the solution again.

Any corrections can then still be made.

Since these measurements are all on a solution of 30 kg of low methylester Pectin in 1,200 1 water (= 2.5%) are practiced when working with differently concentrated solutions should be based on other calorific values. pH and Viscosity measurements are then redefined.

For example, it is possible to use higher pectin concentrations to work, with, for example, 30 kg of pectin in an amount of water of, '00 - 800 1 water can be mixed in. for the subsequent precipitation it is advantageous to a higher concentration than 2,) to choose, for example a 5% pectin solution.

In the case of a positive laboratory test for the pectin preparation solution or

Pectin derivative solution is then the solution in a known manner like in alcohol.

When the precipitation is complete, it is pressed out by means of a screw press.

The pressed pectin derivative is dried at a maximum of 600 C in a stream of air. Then it is ground as usual.

The calcium-phospho-pectin obtained has those described at the beginning beneficial properties.

In addition, experiments were carried out, including the dependence to test the gelation of the initial pH value of the pectin preparation solution. Has it has been shown that at a pH value of approx. 5.0 with a defined CaCl2 content the gelation is best. When the 2.5% pectin preparation solution has a pH above 5.0, the higher the gelling power in the test boil, the worse is the pR value of the initial solution. The pH value in the test boil is constant between 2.9 and 3.0. This experiment is intended to show that at pH values above 5.0 in the pectin solution decreases the gelling power.

Solutions with a pH of 5.0 are in terms of viscosity very thin. In any case, a low pH or a high viscosity is the Solution advantageous, as calcium phosphate is more difficult to settle. One Sufficient phosphating of the preparation or derivative is still guaranteed.

Claims (8)

P a -L P n t a n s p r ü c h e 1. Method for producing a Pectin derivatives based on fruit pectin for the production of jellies with in particular low dry matter content, characterized in that a) A pectin is used as the starting material, which has a metal binding of 30 - 140 mg Metal salt, calculated as CaCl2, per kilogram of pectin for one degree of esterification of 30-40%, preferably 35-38 ', b) at a temperature between 10 and 90 ° C produces such a solution from this pek-tin, water and phosphate that a pH between 4.4-4.8 is obtained, c) the solution is given a certain amount of metal salt adds, and d) the pek-tinderiva-t formed precipitates out of the solution and dries. 2. The method according to claim 1, characterized in that as The starting material used is a pectin, which has a calcium binding capacity of 30 - 140 mg CaCl2 per kilogram of pectin for a degree of esterification of 30 - 40%, preferably 35 -has, and that in step c) an amount of CaCl2 in the form of a solution with vigorous stirring adds to the solution. 3. The method according to claim 1 or 2, characterized in that adding a further amount of phosphate to the solution after adding the metal salt, to achieve a pH value of 5.0 + 0.2. 4. The method according to claim 1 or 2, characterized in that after adding the metal salt, a further amount of phosphate is added to the solution in order to adjust the viscosity to 30-35 cP at 200 C, measured at 2770 s ¹. 5. The method according to any one of claims 1 to 4, characterized in that that the phosphate used is polyphosphates, pyrophosphates, especially Tetranatriurflpyrophosphat, used. 6. The method according to any one of claims 1 to 5, characterized in that that the pectin derivative precipitates with alcohol. 7. The method according to any one of claims 1 to 6, characterized in that that one squeezes the precipitated pectin derivative by means of a screw press. 8. The method according to claim 7, characterized in that the The pressed pectin derivative dries at a temperature not exceeding 600 C.