Lactose crystallisation in ice cream

IntroductIon

Lactose crystallisation is always a risk in ice cream where the lactose content is too high and storage conditions poor. Depending on the amount and size of the lactose crystals that develop, ice cream gains an unpleasant sandy mouthfeel. This Technical Memorandum describes how and why lactose crystals are formed in ice cream, and how this quality defect can be controlled.
Lactose

Lactose exists in two isomeric forms, and , which differ only in the configuration of the substituent on the first carbon atom of the glucose residue. The solubility of the two isomers differs significantly, only 7% w/w -lactose dissolving in 15C water compared to 50% w/w -lactose. Once the lactose is dissolved, mutarotation of the two isomers occurs, yielding a solution that contains approx. 63% -lactose at equilibrium. Sources Traditional ice cream is based on cream or vegetable fat, with skimmed milk powder and whey powder contributing fat-free milk solids. Table 1 shows the approximate composition of the most
raw material

Lactose (milk sugar) is a naturally occurring carbohydrate present in milk and milk products. In ice cream, lactose contributes to mouthfeel and taste through its ability to add bulk, influence on freezing point depression and sweetness. The freezing point depression factor (FPDF) of lactose is 1.0, which means it has the same reducing effect on the freezing point as sucrose, while the relative sweetness is 0.3 compared to 1.0 for sucrose. Chemical properties of lactose Lactose is a disaccharide comprising one D-glucose and one D-galactose unit joined in a -1,4-glycoside linkage as illustrated in figure 1.

common lactose-containing ingredients used in ice cream formulations. A wide variety of tailor-made skimmed milk powder replacers with differing lactose content are available on the market. In order to estimate the total lactose content of a formulation, it is necessary to know the lactose content of the skimmed milk powder replacer. The total lactose content of a recipe can be calculated by multiplying the lactose concentration of each raw material with the amount used (in %) and then adding up the results. Table 2 illustrates three ice cream recipes based on 8% vegetable fat and different sources of MSNF (all the recipes have a MSNF factor of 17).

Lactose %

Protein %

Fat %

Water %

Whole milk Skimmed milk Skimmed milk powder Cream, 38% fat Traditional whey powder Whey protein concentrate 35 Buttermilk powder Evaporated milk Condensed milk

4.5 4.7 50.5 3.0 79.0 51.0 50.0 9.7 11.9

3.4 3.5 36.0 2.2 12.0 35.0 33.0 7.5 7.8

3.5 0.1 1.0 38.0 1.0 3.0 5.0 8.3 8.5

87.8 90.9 4.0 56.4 2.5 5.0 3.5 27.0 30.0

Table 1. The composition of ice cream ingredients.

raw material
OH 3 OH 4 OH 5 O 2 H 1 O OH H 4 OH OH CH2OH O

Formulation a

Formulation B

Formulation c

Coconut oil Skimmed milk powder Whey powder Sucrose Glucose syrup powder Water Total percentage

7.90% 9.50% 2.00% 12.00% 5.00% 63.60% 100.00%

7.90% 5.75% 5.75% 12.00% 5.00% 63.60% 100.00%

7.90% 11.50% 12.00% 5.00% 63.60% 100.00%

6 CH2OH

Figure 1. Chemical composition of lactose.

Table 2. Composition of three ice cream formulations.

TM 2537-1e

In these recipes, only skimmed milk powder and whey powder contain lactose. Thus the total lactose content of formulation A is calculated as 9.50% skimmed milk powder with 50.5% lactose (9.50% x 50.5% = 4.8%) added to 2.0% whey powder with 79.0% lactose (2.0% x 79.0% = 1.6%) giving a total lactose content of 6.4% (4.8% + 1.6% = 6.4%). Using the same formula, the total lactose content of formulation B is 7.4% (5.75% x 50.5% + 5.75 x 79.0% = 7.4%), while formulation C contains 9.1% lactose (11.5% x 79.0% = 9.1%).
Ice cream Phases

60

50

40 Content, % Concentration, %

30

20

10

0.0

-5.0

-10.0

-15.0

-20.0

-25.0

0 -30.0

Temperature,C Air phase Ice crystal phase Lactose concentration in unfrozen water Fat phase Continuous phase

Frozen ice cream consists of four immiscible phases (ice, air, fat and unfrozen continuous phase), where the fat phase and air phase are assumed to be constant after the ice cream has been through the freezer. When the temperature of the ice cream is lowered during hardening, the water in the formulation freezes, creating larger ice crystals. As a result of the ice formation, the unfrozen continuous phase decreases. This is outlined in figure 2, which illustrates the concentration of the four phases in formulation A with 100% overrun. The theoretical content of the four phases is illustrated as a function of temperature. During the ice cream freezing process, the continuous phase becomes more concentrated, causing its viscosity to increase and slowing down the migration of lactose and other sugar molecules in the mix. Figure 2 also illustrates the lactose concentration in the unfrozen water of the continuous phase. The combination of the high lactose concentration and its reduced solubility due to the lower temperature results in a supersaturated lactose solution that contains more sugar molecules than if the system had been in thermodynamic equilibrium.
Lactose crystaLLIsatIon

Figure 2. The concentration of the four ice cream phases during freezing and the concentration of lactose in the unfrozen water during freezing.

Lactose crystallisation is the process of formation of solid crystals from a solution. Crystallisation happens in two steps:

nucleation and crystal growth. Nucleation occurs when dissolved molecules of solute lactose aggregate and form stable nuclei. The second step, crystal growth, follows when these nucleus start to grow. Crystallisation can be divided into primary and secondary crystallisation. Primary crystallisation is the nucleation of a crystal, for example, from a cluster of lactose (homogeneous crystallisation) or by using other seeding materials in the solution (heterogeneous crystallisation). Homogeneous crystallisation generally takes place in pure systems in the absence of any foreign particles. In practice, heterogeneous crystallisation is the primary mechanism and it is initiated by solid particles of impurities in the ice cream. Secondary or forced crystallisation refers to the process of nuclei formation due to crystal fragments already present in the solution. These fragments can result from agitation, pumping or other kinds of mechanical treatment, where dendrite-shaped crystals can break up. Because -lactose is much less soluble than -lactose at low temperature, -lactose crystallises, causing the solution to become less supersaturated. This
2

results in mutarotation of -lactose to -lactose in order to maintain equilibrium. When more -lactose is formed, the solution becomes supersaturated, and more -lactose crystallises. The crystals that form are mainly -lactose, providing the mutarotation rate is sufficiently high compared to the crystallisation rate. -lactose tends to form wedge or tomahawk-shaped crystals (see figure 3). The -lactose crystal only grows in one direction from the apex of the tomahawk, and does not show the multidirectional growth of, for example, sucrose crystals. Research has suggested that the average crystallisation velocity of the single active side of the tomahawkshaped crystal is comparable to that of a sucrose crystal, possibly explaining the slow growth rate of -lactose crystals. The sharp edges of the tomahawkshaped crystals make them extremely unpleasant in the mouth when they reach a certain size. It is widely recognised that the critical size of tomahawk-shaped lactose crystals is around 15m for detection in the mouth. By way of comparison, ice crystals have a detection limit of 50m in the mouth. The difference in the detection limits of the two crystal types

Figure 3.Tomahawk-shaped lactose crystals in bright field optical microscopy using white light (A) and polarised light (B).

is partly the crystal shape and partly the fact that lactose crystals do not dissolve in the mouth. This makes it easy to distinguish lactose crystals from ice crystals in ice cream, as ice crystals melt (disappear) in the mouth whereas lactose crystals do not.
Factors InvoLved In Lactose crystaLLIsatIon

In practice, lactose crystallisation is a consequence of the ice cream formulation and storage temperature. It is widely accepted that, if the total content of lactose exceeds 10% of the water in the ice cream mix, then the risk of lactose crystallisation is high. In the example used in this paper, the total solids content of the three formulations is 34.7%, which means the lactose content should not exceed 6.5% (10% x (100% - 34.7%)). The total lactose content of formulation A is 6.4%, giving a low risk of lactose crystallisation. The risk is higher with formulation B, where the total lactose content is 7.4%. Formulation C contains 9.1% lactose, which is highly likely to result in lactose crystallisation. The rate of lactose crystallisation is primarily controlled by two competing mechanisms. As the amount of water decreases in the continuous phase during freezing, the supersaturation of lactose goes up, leading to increased lactose crystallisation. However, when the amount of frozen water goes up, the viscosity of the continuous unfrozen phase starts to increase, inhibiting lactose crystallisation due to the lower molecular mobility of the phase. The increased

viscosity can be manipulated by the use of specific hydrocolloids. The speed of crystallisation is temperature dependent, explaining why decreasing temperatures slow the growth rate of lactose crystals. Previous research has indicated that the practical maximum growth rate and lowest induction time for nucleation of lactose crystals in standard ice cream is around -10C to -12C, depending on the freezing point depression of the recipe (see figure 4). Lactose crystallisation is substantially decreased as the temperature of the continuous phase moves towards the glass transition phase (approximately -30C). The mutarotation of -lactose to -lactose is dependent on temperature. This reduces the crystallisation rate at low temperatures. Factors such as

14 12 Induction time, h 10 8 6 4 2 0 -25 -20 -15 -10 -5 0

pH and a high concentration of other sugar molecules and salts also have a negative influence on the mutarotation of -lactose to -lactose, thus enhancing the inhibition of lactose crystallisation at low temperatures. As -lactose appears to inhibit the growth of -lactose crystals, it is important for lactose crystallisation that mutarotation occurs. Experiments have shown that additives that work as nuclei for lactose crystallisation can also prevent sandiness by promoting a high number of tiny lactose crystals. The crystals are then naturally smaller in size and, if enough nuclei are added, can be maintained below 15m. Microcrystalline cellulose is one of the additives suitable for nucleation and can be used in formulations where lactose crystallisation is a potential problem. It has also been shown that the addition of smaller amounts of particles that can act as lactose crystal nucleation sites can dramatically speed up the development of sandy textures in ice cream. This is often the case with chocolate, cookie, nut paste or cake inclusions. Additives, impurities or conditions can interfere significantly with lactose crystallisation, for example, by altering the conditions of the equilibrium solution, adjusting the viscosity of the continuous phase, promoting or inhibiting nucleation, or changing the growth rate or shape of the crystals. However, the main factors involved in lactose crystallisation are a critically high lactose content and the storage temperature of the ice cream.
PreventIng Lactose crystaLLIsatIon

Temperature, C

Figure 4. Dependence of induction time for nucleation on storage temperature; sinusoidal thermal fluctuations of +/-1.0C with a 10-min. cycle time. Source: Influence of temperature on crystallization of lactose in ice cream,Yoav D. Livney, Daniel P. Donhowe & Richard W. Hartel, International Journal of Food Science and Technology (1995) 30, page 311-320. 3

The presence of lactose crystals in ice cream results in a sandy, gritty mouthfeel, regarded as a quality defect. As described, lactose crystals only appear in ice cream if the formulation contains excessive lactose and is subject to poor storage and distribution conditions. Therefore, the best way to control lactose crystallisation is to focus on the recipe and storage temperature.

danisco a/s Edwin Rahrs Vej 38 DK-8220 Brabrand, Denmark Telephone: +45 89 43 50 00 Telefax: +45 86 25 10 77 info@danisco.com www.danisco.com

The information contained in this publication is based on our own research and development work and is to the best of our knowledge reliable. Users should, however, conduct their own tests to determine the suitability of our products for their own specific purposes and the legal status for their intended use of the product. Statements contained herein should not be considered as a warranty of any kind, expressed or implied, and no liability is accepted for the infringement of any patents.

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