Ultrasonic characterization of lactose dissolution

The ultrasonic properties (at 2.25 MHz) of lactose solutions and suspension of lactose crystals (d ∼ 50 μm) were measured as a function of concentration (0–40 wt.%). Ultrasonic velocity increased linearly with concentration regardless of the state of dissolution of the lactose crystals while ultrasonic attenuation was low and concentration-independent when the lactose was dissolved and increased approximately linearly with the concentration of suspended crystals. Therefore the amount of lactose present and the state of dissolution can be determined simultaneously with single ultrasonic sensor. A sensor based on this principle was applied to a stirred tank and used to measure the time taken to mix powdered lactose into a solution and the time for the added lactose to dissolve.     

Crystallization and X-ray Diffraction of Crystals Formed in Water-Plasticized Amorphous Spray-dried and Freeze-dried Lactose/Protein Mixtures

ABSTRACT: Effects of proteins (whey protein isolate [WPI], Na-caseinate, and gelatin), drying method, storage relative vapor pressure (RVP), and time on lactose crystallization and crystals formed were investigated using x-ray diffraction (XRD). Crystallization was observed from increasing peak intensities of XRD patterns. Lactose in lactose/protein (5:1,3:1) mixtures crystallized in samples stored at RVP of 44.1% and above in both spray-dried and freeze-dried materials, except in freeze-dried lactose/Na-caseinate and lactose/gelatin mixtures, which showed lactose crystallization at 54.5% RVP and above. The rate of crystallization increased with increasing RVP and storage time. The rate of crystallization in spray-dried materials was higher than in freeze-dried materials, and the crystallization rate decreased with increasing protein content. Lactose crystallized mainly as α-lactose monohydrate in spray-dried lactose/WPI and lactose/gelatin mixtures. Crystals formed in freeze-dried lactose/WPI and lactose/gelatin mixtures were anhydrous β-lactose and α-lactose monohydrate crystals. Lactose crystallized as a-lactose monohydrate in both spray-dried and freeze-dried lactose/Na-caseinate mixtures. Trace amounts of anhydrous β-lactose were present in spray-dried lactose/WPI (5:1) and lactose/gelatin (5:1) mixtures. Peak intensities of XRD patterns for anhydrous β-lactose decreased with increasing protein content and storage time. The crystallization data were successfully modeled using Avrami equation at an RVP of 65.6% and above. These data are important in understanding and predicting storage stability of lactose- and protein-containing food and pharmaceutical materials.     

Ultrasonic monitoring of lard crystallization during storage

This work addresses the use of ultrasonics as a non-destructive technique with which to monitor lard crystallization during cooling and storage. The ultrasonic velocity was measured during both the isothermal crystallization of lard (at 0, 3, 5, 7, 10 and 20 °C) and during the non-isothermal crystallization. In addition, lard crystallization was also studied through Differential Scanning Calorimetry (DSC) and instrumental texture analysis (penetration tests). The measurement of the ultrasonic velocity allowed the bulk crystallization to be detected. The evolution of the ultrasonic velocity and the textural measurements during isothermal crystallization showed two steep increases, which may be explained by the two fractions of triglycerides found in DSC thermograms. At 7, 10 and 20 °C the second fraction did not crystallize within the first 11 days of storage. A two-step crystallization model based on the Avrami model was used to properly describe (% var > 99.9 and RMSE < 1.99 m s^− 1) the relationship between the ultrasonic velocity and the isothermal crystallization time. In addition, a model was developed to estimate the percentage of solid fat content during isothermal crystallization. Therefore, it may be pointed out that ultrasonic techniques could be useful to monitor the crystallization pattern of complex fats during long periods of storage.     

In Situ Ultrasonic Characterization of Cocoa Butter Using a Chirp

Differences between tempered and untempered cocoa butter were investigated by an ultrasonic signal “chirp” generated by contact transducers. Polarized light microscopy and powder X-ray diffraction were used to characterize the morphology and polymorphism of tempered and untempered cocoa butter, whereas pulsed nuclear magnetic resonance was used to determine the amount of crystalline solids present. Ultrasonic wave velocity and attenuation data were collected simultaneously throughout the 5-h crystallization process for cocoa butter. Ultrasonic velocity and attenuation changed at the different solid fat contents (SFC): 4, 8, and 11 %. Untempered cocoa butter showed an attenuation of 3 dB/cm at 1.7 MHz and 4 % SFC, whereas tempered cocoa butter showed an attenuation of 4.5 dB/cm at 1.7 MHz and 4 % SFC. At 3 MHz, the attenuation was 2 dB/cm for untempered and 6 dB/cm for tempered cocoa butter. Under these conditions (4 % SFC, 3 MHz), the chirp wave of tempered sample showed a phase angle change of 0.5 rad, whereas the untempered sample showed ?0.5 rad relative to the canola oil that was taken as 0. The study suggests that an ultrasonic chirp can be effectively used to detect differences between tempered and untempered cocoa butter when measuring attenuation and ultrasonic wave phase angle changes as a function of frequency. The in-line characterization of chocolate “temper” using such nondestructive ultrasonic measurements could be applied to industrial chocolate manufacturing.     

Water Sorption and Plasticization Behavior of Spray-dried Lactose/Protein Mixtures

ABSTRACT: Water sorption properties, effects of proteins on glass transition temperature, and time-dependent lactose crystallization of spray-dried lactose and lactose in lactose/WPI (3:1), lactose/Na-caseinate (3:1), lactose/albumin (3:1), and lactose/gelatin (3:1) mixtures were investigated. Brunauer-Emmett-Teller (BET) and Guggenheim-Anderson-de Boer (GAB) models were used to model water sorption. Lactose/protein mixtures sorbed high amounts of water at low relative vapor pressure (RVP) up to 23.1%. Above 23.1% RVP levels, water sorbed by pure lactose was higher, up to 44.1% RVP, except in the case of the lactose/gelatin mixture. Lactose/ gelatin also sorbed a high amount of water at 33.2% RVP. Loss of sorbed water resulting from crystallization of amorphous lactose was observed. Crystallization of pure lactose and lactose crystallization in lactose/protein mixtures occurred at RVP ≥ 44.1% within 24 h. After crystallization at RVP ≥ 54.5%, water contents remained higher for lactose/protein mixtures than for pure lactose. The rate of lactose crystallization was less in all lactose/protein mixtures than was observed for pure lactose. WPI had the lowest effect on lactose crystallization. Crystallization occurred most slowly in lactose/gelatin mixtures. Both GAB and BET models fitted to water sorption data up to 0.441 a_w. It seems that different proteins interact with lactose differently. Water sorption and time-dependent lactose crystallization of lactose/protein mixtures have important consequences to processing and storage behavior of lactose-protein based products.     

Nonenzymatic Browning Kinetics in Low-moisture Food Systems as Affected by Matrix Composition and Crystallization

ABSTRACT: Nonenzymatic browning (NEB) in lactose, trehalose, and lactose/trehalose food model systems containing L-lysine and D-xylose (5% w/w) as reactants was studied at 4 different relative vapor pressure (RVP) (33.2%, 44.1%, 54.5%, 65.6%) environments at room temperature. Sorption isotherms of model systems were determined gravimetrically, and data were modeled using the Brunauer-Emmett-Teller (BET) and Guggenheim-Anderson-deBoer (GAB) models. Glass transition, T_g , was measured by differential scanning calorimetry (DSC). NEB was followed spectrophotometrically. Although the 3 model systems showed similar glass transition behavior, different crystallization properties were observed from loss of sorbed water. Mixtures of trehalose and lactose showed delayed crystallization of component sugars. The NEB rate was affected by sugar composition. At a low RVP (33.1%) environment, the NEB rate in trehalose system was higher than in the lactose/trehalose system, and the NEB rate in lactose system was the lowest. The NEB rate in different models seemed to be affected by component crystallization. The highest extent of browning in the trehalose matrix system seemed to be related to the formation of trehalose crystals in the system after crystallization at high RVP. The results indicated that the composition of the carbohydrate-based low-moisture real food systems should be considered in controlling NEB reaction.     

超声波技术在食品工业中的最新应用进展

综述声化学中超声波技术在食品工业的应用状况。超声波技术在食品工业中的分析检测和改性领域得到越来越广泛的应用。低强度的超声波技术为一非破坏性技术 ,可用来分析检测食品体系中一些非常有用的物化性质 ,如组成 ,质构 ,流变学性质等。高强度超声波技术主要被用于食品的物理和化学改性领域 ,如嫩化肉 ,促进乳化 ,加快化学反应 ,钝化酶及加速溶液起晶 ,提高大豆蛋白质的浸提率等     

Structural strength and crystallization of amorphous lactose in food model solids at various water activities

Freeze-dried lactose and lactose/whey protein isolate (WPI) mixtures were used as amorphous food models at various a_w, and the effects of temperature and water and WPI contents on physical state were analyzed. Thermal behavior and mechanical properties were studied and Williams-Landel-Ferry (WLF) model was fitted to structural relaxation times (τ). The WLF-analysis gave a strength parameter (S) that was used to describe structural strength of the food solids. Our results showed that lactose and WPI in mixtures exhibited fractional water sorption. Thermal properties and structural strength of the solids were affected by water and WPI while T_g measured for the lactose/WPI systems followed that of the lactose component and showed phase separation of lactose and proteins. A relationship between S and water content was established, whereas the crystallization of amorphous lactose was more rapid in systems with a smaller S. Therefore, S provided a simple and convenient measure of τ controlling structure formation in food processing as well as to control lactose crystallization.Industrial relevanceSugars are common ingredients and often used as a mixture with other components, e.g., proteins, in the food and pharmaceutical industries. Thus, understanding the physical state and thermal behavior of sugar containing food materials has a great importance in the development of processing and shelf life control procedures for such ingredients and relevant products. This study provides physicochemical information about thermal and mechanical properties of freeze-dried lactose/whey protein systems used as food models at various water activities. Data on water sorption, time-dependent lactose crystallization, calorimetric glass transition and crystallization temperatures, and structural relaxation times can be used to understand and predict structural changes during processing and storage of relevant foods. Moreover, the structural strength concept, described in this study, allows of the control of crystallization behavior as a physical state and time-dependent phenomenon, and therefore, stability of food and pharmaceutical materials     

Cover Caption

On the cover : Micrograph of lactose crystals in a gelatin gel, from “Ultrasonic Characterization of Lactose Crystallization in Gelatin Gels” by John Coupland and Umut Yucel; p E49.     

Water Plasticization and Crystallization of Lactose in Spray-dried Lactose/Protein Mixtures

ABSTRACT: Water plasticization led to depression of the glass transition causing significant changes in the physico-chemical and crystallization properties in storage of lactose and lactose/protein (3:1) mixtures. Glass transition (Tg) and crystallization temperatures (Tcr) were determined using differential scanning calorimetry. Whey protein isolate (WPI), albumin, and gelatin increased the Tg of dry powders; when Na-caseinate was used, a decrease was observed. In the presence of proteins and water, a decrease of Tg at aw ≤ 0.23 was observed. At aw ≤ 0.33, proteins increased the Tg In the anhydrous state, Tcr decreased in the presence of proteins possibly because of browning. WPI, Na-caseinate, albumin, and gelatin delayed lactose crystallization in humidified samples, with albumin and gelatin delaying it more than WPI at all storage humidities. Temperature difference between an observed instant crystallization and glass transition (Tcr to Tg) was larger for humidified samples containing proteins than for lactose. Various proteins and water affect crystallization behavior of amorphous lactose differently in spray-dried powders. This should be considered in evaluating sugar crystallization properties in food products including dairy powders.     

Monitoring Tempered Dark Chocolate Using Ultrasonic Spectrometry

Ultrasonic spectrometry was used to distinguish between properly tempered and untempered commercial dark chocolate. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) were used to characterize the polymorphic state of tempered and untempered chocolate, results that were correlated to those of ultrasonic spectrometry. Four different kinds of dark chocolate samples with different amounts of sugar (7.5–50 %), fat (30–50 %), and cocoa mass (70–90 %) were subjected to two different tempering protocols. The tempering was achieved using cocoa butter seeds under static cooling from 50 to 14 °C. The ultrasonic generator and analyzer SIA-7 (V.N. Instruments) was used to monitor the crystallization process. The instrument generated a chirp signal with a bandwidth of 0.5 to 3 MHz and was set to work in a four-pathway configuration with two transducers and a center frequency of 2.25 MHz. Spectrometric analysis was carried out with chocolate samples containing 2, 4, and 6 % solid fat content (SFC). The SFC was obtained from DSC measurements. Ultrasonic signals for attenuation, reflection, and velocity were compared between tempered and untempered chocolates. It was shown that seed-tempered chocolate with 30 % sugar and 47.5 % fat attenuated 2.5 MHz of ultrasonic waves by 0.8, 1.7, and 2.0 dB/cm at 2, 4, and 6 % SFC, respectively. On the other hand, untempered chocolate attenuated the ultrasound signal by 3.5, 3.6, and 4.3 dB/cm. Furthermore, it was found that ultrasound reflection signals were stronger and ultrasonic velocity was higher in chocolates with high sugar content.     

An Ultrasonic Method for Assessing the Residence Time Distribution of Particulate Foods During Ohmic Heating

ABSTRACT: The residence time distribution (RTD) was investigated using ultrasound during continuous ohmic heating of 1) starch solution and 2) carrot particles/starch solution mixtures. For liquid experiments, a copper pigment was used as a tracer. Ultrasonic sensors were placed at the end of the tube to measure changes in sound attenuation. The copper concentration was determined in samples taken at time intervals. For particulate foods, one kilogram of carrot/solution mixtures was introduced. Results of the ultrasonic method were compared to carrots weights in collected samples. Variations of sound attenuation illustrated well the RTD of solutions and carrot particles. Results of the ultrasonic method agreed with the pigment method for liquid and the gravimetric method for particulate foods.     

DETERMINATION OF ULTRASONIC‐BASED RHEOLOGICAL PROPERTIES OF DOUGH DURING FERMENTATION1

An ultrasonic technique was used to study the changes of the rheological properties of dough during fermentation at 37C and compared with the extensional properties of fermented dough obtained from tensile tests carried out in a Universal Testing Maching. The velocity and attenuation of a longitudinal wave (P‐wave) propagated through the dough samples were measured and analyzed to obtain the viscoelastic moduli of the dough; the storage modulus M' and the loss modulus M''. These moduli include both the bulk and the shear moduli. A wavelet analysis also was used to determine the effect of frequency on the ultrasonic‐based viscoelastic moduli and the effect of the fermentation process on the ultrasonic velocity dispersion. A decrease in ultrasonic velocity was observed with increasing fermentation times. Ultrasonic waves were strongly attenuated in the dough subjected to long fermentation times and fermentation had a large influence on the viscoelastic moduli of the dough. The ultrasonic velocity increased with increasing frequency, clearly showing the viscoelastic nature of the fermented dough. The analysis also showed significant ultrasonic velocity dispersion upon fermentation. Ultrasonic measurements yielded results that agreed with those obtained from conventional rheology commonly used to characterize the extensional properties of dough. Both tests clearly showed the loss of elasticity by the dough samples upon fermentation.     

Insight in ultrasonic shear reflection parameters by studying temperature and limonene influence on cocoa butter crystallization

In this study an inverse model was developed to derive relevant ultrasonic parameters from ultrasonic shear reflectometry measurements. The inverse model includes four variable parameters: t_ind (induction time), K (crystallization rate), v_s2 (shear ultrasonic velocity) and a_s2 (shear ultrasonic attenuation coefficient). Both the temperature effect and the effect of a minor component limonene (in different concentrations) on the isothermal crystallization of cocoa butter were studied with the ultrasonic shear reflectometry technique and associated inverse model. Subsequently, the ultrasonic parameters were compared with results of conventional techniques to monitor fat crystallization (DSC, PLM). The study shows that t_ind and K provide information on the kinetics of the microstructure development. The parameter v_s2 is related with the equilibrium SFC, while a_s2 is both influenced by the SFC and the organization of the crystals in the network, yielding information about the microstructure of the crystallized samples.Industrial relevanceThe microstructure of crystallized fat determines to a large extent the macroscopic properties of fat rich products, such as texture, mouthfeel,… Hence, monitoring the crystallization behavior (including not only the primary crystallization but also the microstructural development) during the production process is of utmost importance in order to obtain high quality end products. The ultrasonic shear reflectometry technique is a fast non-destructive technique which provides quantitative data about the crystallization process based on an inverse model. The simplicity of the technique offers potential for inline control. This may be beneficial to evaluate the crystallization process under different process conditions and to stimulate product innovation as more insight can be obtained in the microstructure development of new products.     

Rates of Crystallization of Dried Lactose-sucrose Mixtures

The isothermal crystallization kinetics of glassy lactose/sucrose mixtures were studied at several storage temperatures (close to T_g and T_m). The kinetic parameters implicit in the Avrami equation were determined. Activation energies for transport (E_D) and surface nucleation (W*) were also found and correlated to the molar composition of the lactose/sucrose mixtures. A monotonic increase in the half crystallization time (t_1/z), Avrami index (n), % crystallization per day, activation energy for transport (E_D) and surface nucleation energy (W*) and a decrease in the crystallization velocity constants (K) were related to the increase in the lactose content of lactose/sucrose mixtures.     

Crystallization behavior of lactose/sucrose mixtures during water-induced crystallization

The crystallization behavior of lactose/sucrose mixtures during water-induced crystallization was studied to gain more insight about their crystallization during storage. Solutions with different ratios of lactose and sucrose, 75:25 and 50:50, were spray dried to produce amorphous powders. The powders were kept at a controlled temperature and humidity to study their sorption–desorption behavior. X-ray diffraction and light microscopy analysis were performed to study their crystallization behavior. Two-step desorption was observed after sieving the powders as sample preparation. Sieving decreased the crystallization time for lactose/sucrose mixture 75:25 from 22 days to 2.5 days. Based on the X-ray diffraction analysis during this two-step process of water desorption, it was concluded that lactose crystallizes first and more quickly than sucrose. The degree of crystallization for the lactose crystals increases by 89% (relative to their final level of crystallinity), whereas sucrose crystals increase their level of crystallinity by only 28% during the first step of crystallization in the lactose/sucrose (75:25) mixtures. The light microscopy images also suggested that the crystallization of amorphous lactose/sucrose powders during water-induced crystallization may occur as a solution rather than in the solid phase.     

Lactose crystallization delay in model infant foods made with lactose, beta-lactoglobulin, and starch

Handling and storage alter infant food powders due to lactose crystallization and interactions among components. Model infant foods were prepared by colyophilization of lactose, β-lactoglobulin (β-LG), and gelatinized starch. A mixture design was used to define the percentage of each mixture component to simulate a wide range of infant food powders. The kinetics of crystallization was studied by a gravimetric method (dynamic vapor sorption) at 70% relative humidity (RH). After freeze-drying, lactose was amorphous and crystallized at 70% RH. The delay before crystallization depends on the contents of β-LG and starch in the formulations. A mathematical model was proposed to predict crystallization time (delay) at 70% RH. For the formulation containing 50% lactose, 25% β-LG, and 25% starch, lactose was still amorphous after 42 h at 70% RH, whereas pure amorphous lactose crystallized after approximately 70 min. Calculated and experimental results of adsorbed moisture from the formulations were compared. Adsorbed water of formulation containing lactose could not be calculated from moisture sorption properties of each component at a given RH because β-LG and gelatinized starch prevented lactose crystal growth.     

牛奶中主要成分超声特性及温度影响的研究

用超声波测量牛奶中主要成分含量的方法是基于超声特性参数与溶液组分的关系,这种关系还受到温度的较大影响。本实验研究了超声波的速度(衰减)与牛奶中主要成分含量以及温度的关系。结果表明,在温度为30～50℃范围内,牛奶中的声速随温度升高先增加后减小,衰减则随温度升高而增加;在同一温度下,声速和衰减随时间无显著改变。根据实验结果计算出牛奶中脂肪和蛋白质与声速(衰减)之间的关系,为完善检测方法和检测系统提供了参考。     

α-Relaxation in honey study versus moisture content: High frequency ultrasonic investigation around room temperature

Ultrasonic longitudinal attenuation and velocity have been measured for various frequencies between 0.5 and 13.5 MHz versus temperature, in honeys with moisture contents between 15% and 19%. With the help of attenuation measurements, the temperature of the alpha transition T_α (associated with the glass transition) has been deduced versus moisture content and ultrasonic frequency. Regarding the high sensitivity of T_α towards moisture content, one can distinguish two honeys with moisture contents difference less than 0.1%. Considering the fact that the experiments are not difficult to perform and are carried out at around room temperature, this technique could be useful for honey quality control or more generally for aqueous polymers study.     

Non-contact ultrasonic measurements in food materials

A novel air-coupled transducer and signal generator is used to measure the speed of sound and thickness (5–15 mm) of samples of various food products (cheese, reduced fat cheese, luncheon meat, reduced fat luncheon meat, and cranberry sauce). Measurements were made with two transducers (1 MHz) placed one either side of the sample at a distance of approximately 30 mm from the food surface. Thicknesses measured by this method were similar to measurements made using calipers for all samples. At a single point the ultrasonic measurements were very precise (s.d. 0.003 mm, n=12) but when several points on the same slice were averaged the precision reflected unevenness in the slicing operation. Ultrasonic velocity measurements were made using non-contact and conventional contact-mode ultrasound. The precision of both methods was similar but the apparent speed of sound measurements made in contact mode were significantly higher, suggesting the soft solids studied were compressed during analysis.