Glass transition and flowability/caking behaviour of maltodextrin DE 21

Maltodextrin DE 21 is a spray dried amorphous powder that is commonly used as an ingredient in the food industry. The powder or an ingredient mix containing the powder can form very strong cakes if exposed to certain consolidating pressures and climatic conditions. In particular, it was believed that the glass transition can influence its caking behaviour. Consequently, the focus of this study was to investigate the influence of exposing maltodextrin DE 21 powder to temperatures around its glass transition and to measure its flowability or cake strength using a ring shear tester. To enable this work, the influence of water content on the onset glass transition temperature was measured along with the sorption isotherm of the powder. The ring shear testing showed that the maltodextrin powder readily formed a very strong cake over time when it was exposed to temperatures that were at or above its onset glass transition temperature. Maintaining the powder temperature at 4 °C below its glass transition should prevent the powder from caking.     

Milk powders ageing: effect on physical and functional properties

Milk powders are now considered as food ingredients, mainly because of the functional properties of milk proteins. During the storage of milk powders, many physicochemical damages, mainly dependent on lactose glass transition occur. They have important consequences on physical (flowability) and functional properties (solubility, emulsifying, and foaming properties) of milk powders. First, lactose crystallization modifies the microstructure and chemical composition of the surface of powder particles. Thus, milk powders flowability is decreased. Since the structure of milk proteins is destabilized, its solubility is damaged. Moreover, particle collapse and caking occur and mainly decrease the physical properties of milk powders (density and flowability). The mechanical stresses involved may also enhance proteins unfolding, which is detrimental to solubility. Finally, molecular mobility is favored upon ageing, and both chemical (Maillard reaction) and enzymatic reactions occur. Maillard reaction and oxidation enhance protein interactions and aggregations, which mainly lessen milk powders solubility. Maillard reaction also decreases emulsifying and foaming properties. Storage temperature and relative humidity have been considered as the predominant factors involved, but time, milk components, and their physical state also have been implied.     

Moisture-induced caking of beverage powders

BACKGROUND: Beverage powders can exhibit caking during storage due to high temperature and moisture conditions, leading to consumer dissatisfaction. Caking problems can be aggravated by the presence of sensitive ingredients. The caking behaviour of cocoa beverage powders, with varying amounts of a carbohydrate sensitive ingredient, as affected by climate conditions was studied in this work. Sorption isotherms of beverage powders were determined at water activities (a_w) ranging from 0.1 to 0.6 in a moisture sorption analyser by gravimetry and fitted to the Brunauer–Emmett–Teller (BET) or the Guggenheim–Anderson–de Boer (GAB) equation. Glass transition temperatures (T_g) at several a_w were analysed by differential scanning calorimetry and fitted to the Gordon–Taylor equation. Deduced T_g = f(a_w) functions helped to identify stability or caking zones. Specific experimental methods, based on the analysis of mechanical properties of powder cakes formed under compression, were used to quantify the degree of caking. Pantry tests complemented this study to put in evidence the visual perception of powder caking with increasing a_w. RESULTS: The glass transition approach was useful to predict the risks of caking but was limited to products where T_g can be measured. On the other hand, quantification of the caking degree by analysis of mechanical properties allowed estimation of the extent of degradation for each product. CONCLUSION: This work demonstrated that increasing amounts of a carbohydrate sensitive ingredient in cocoa beverages negatively affected their storage stability. Copyright © 2011 Society of Chemical Industry     

Caking and Stickiness of Dairy-Based Food Powders as Related to Glass Transition

The effects of heating rate, storage temperature and water activity on surface caking (T_sc) and advanced caking (T_ac) of several dairy-based infant formula powders were determined by the modified ampule and sealed glass test tube methods, respectively. The glass transition temperature, T_g, was determined by differential scanning calorimetry. Observed T_sc and T_ac values were higher at faster scan rates (5 and 10°C/min) compared to a slower heating rate (1°C/3 min). In addition, because of the sample size and the difference in viscous flow time constants, T_ac≥ T_sc≥ T_g. As expected, stability towards collapse and sticking decreased with Increasing amounts of low-molecular-weight carbohydrate. The predicted stable storage water activities at room temperature based on T_sc were higher than those observed during storage; however, the water activity at which T_starage= T_g gave a good prediction of the %RH when collapse begins.     

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.     

Water sorption and glass transition properties of spray dried lactose hydrolysed skim milk powder

The moisture sorption behaviour and glass transition temperature of spray dried skim milk powder with hydrolysed lactose (SMPHL) were determined. Spray drying of skim milk with hydrolysed lactose resulted in very low cyclone recovery of 25% and a large amount of powder remained stuck inside the spray dryer. The equilibrium moisture content of SMPHL was lower than that of lactose for each range of water activity when humidified for 21 days at 23 °C using saturated salt solutions. Unlike lactose, SMPHL did not lose water when the water activity exceeded 0.432 and no crystallization was noticed at water activity ?0.753. The sorption isotherm data for SMPHL fitted well with the BET and GAB models with monolayer moisture contents of 7.55 and 8.27 g/100 g, respectively. The glass transition temperature of anhydrous SMPHL was 49 °C. The critical water activity and moisture content for SMPHL were 0.15 and 2.4 g/100 g dry solid, respectively. The low critical values indicated hydrolysis of lactose necessities maintenance of very low moisture of powder for its long-term stability.     

Ultrasonic characterization of lactose crystallization in gelatin gels

Ultrasonic velocity and attenuation measurements (2.25 MHz center frequency) were used to follow bulk crystallization of lactose (43% and 46%) from gelatin (1.5% and 3%) gels at 25 °C, and compared to turbidity (500 nm) and isothermal calorimetric measurements. Ultrasonic velocity decreased slightly (approximately 0.5%) during crystallization while ultrasonic attenuation was low in the absence of lactose crystals and increased progressively during crystallization. The lag time before the onset of crystallization decreased and the maximum rate of increase in attenuation during crystallization increased with increasing lactose supersaturation but was not affected by gelatin concentration (P < 0.05). Similar results were seen in turbidity and isothermal calorimetric measurements. Ultrasonic attenuation measurements have the potential to measure crystallization kinetics in complex food matrices and to be applied on-line. Practical Application: Many foods contain crystals that affect their taste and texture (for example, lactose crystals can give a grainy defect in ice cream). The formation of crystals is often hard to predict so methods to measure the development of crystals inside real foods are useful. In this study, we show that as lactose crystallizes in a gelatin gel the ultrasonic attenuation--capacity to absorb sound--increases and can be related to the amount of crystals present. Ultrasound is easier to apply in real food processing than the existing methodologies.     

Glass transition phenomena in molasses

Glass transition phenomena were investigated in molasses obtained from five Australian sugar mills. The transition temperatures (midpoint), T_g, ranged from −75 to −35 °C, while the change in heat capacity was from 0.68 to 0.84 J/g⁻¹/°C. The five molasses varied in moisture, sugars and acidity, and this variation affected the T_g. The predicted T_g of the anhydrous form from the models of Fox, Pochan-Beatty-Hinman and Fried, and from a linear model shows that the molasses with the highest moisture gave the lowest transition temperature. The glass transition parameters of anhydrous sucrose, glucose and fructose did not accurately predict the transition temperatures of the molasses.     

Glass transition temperatures and some physical and sensory changes in stored spray-dried encapsulated flavors

Commercial spray-dried powder flavors (strawberry and orange) encapsulated in different amorphous matrices (maltodextrin and maltodextrin-sucrose) were stored for 20 days under constant relative humidities of 32%, 43%, 58% and 75%. Glass transition temperatures (T_g) of the different powders and maltodextrin DE 12 were measured using differential scanning calorimetry (DSC). Caking/collapse visual observations and aroma strength (measured by a trained sensory panel) were recorded and correlated with the glass transition temperature of the different spary-dried flavors. Glass transition data explained collapse occurrence and loss of aroma strength in encapsulated strawberry and orange flavors after storage at various relative humidities.The presence of sucrose in the carrier formulation negatively affects storage stability of the encapsulated flavor.     

Modeling of lactose crystallization and color changes in model infant foods

Lactose crystallization and color changes in formulas containing β-lactoglobulin and gelatinized starch were investigated. Model infant formulas were prepared by colyophilization of 3 components (lactose, β-lactoglobulin, and gelatinized starch). A mixture design was used to choose the percentage of each mixture component. These formulas were stored for 3 mo at different relative humidities (RH), ranging from approximately 0 to 94.6%, to study the lactose crystallization and color changes. Crystallization kinetics was studied by gravimetric methods, and lactose state (crystalline vs. amorphous) was verified before and after storage by differential scanning calorimetry. Before storage, lyophilized lactose was amorphous, but during storage it crystallized, depending on the RH. The lactose crystallization RH depended on the quantity of β-lactoglobulin and gelatinized starch, and by increasing these quantities, the crystallization RH increased. For some formulas, the crystallization RH was noted at 3 different RH during storage. The first was noted after 1 d of storage and the second and third were observed later on, showing that crystallization is a time-dependent phenomenon. Nonenzymatic browning was studied in model infant formulas by yellow color changes of samples at 11.3, 43.2, 54.5, and 75.4% RH. In this study, 7 mathematical models were proposed to predict the moisture sorption properties and color changes at different RH, and the models were validated by experimental results.     

Feeding lactose to increase ruminal butyrate and the metabolic status of transition dairy cows

Twenty-four multiparous Holstein cows (775 ± 24 kg body weight; 3.4 ± 0.11 body condition score) were used in a randomized complete block design experiment to determine the impact of increased ruminal butyrate from the fermentation of lactose on metabolism and lactation. Dietary treatments were either a corn-based control diet (CON) or a diet containing lactose at 15.7% of diet dry matter (LAC). Experimental diets were fed from 21 d before expected calving through 21 d in milk (DIM). Blood was sampled at −21, −14, −7, −2, 2, 7, 14, and 21 DIM, rumen fluid at −21, −7, and 7 DIM, and liver tissue via biopsy at 7 and 14 DIM. Pre- and postpartum dry matter intake (DMI) through 28 DIM averaged 12.8 and 17.7 kg/d, respectively, and did not differ between treatments; however, cows fed LAC did not exhibit a prepartum decrease in DMI. Milk yield was unaffected by treatments and averaged 45.7 kg/d during the first 70 DIM. Plasma glucose, insulin, and non-esterified fatty acids were not affected by dietary treatments. Feeding LAC increased the ruminal proportion of butyrate both pre- (11.3 vs. 9.2 ± 0.45%) and postpartum (13.0 vs. 10.3 ± 0.67%). Likewise, circulating plasma β-hydroxybutyrate was increased both pre- (6.1 vs. 4.2 ± 0.31 mg/dL) and postpartum (14.6 vs. 8.34 ± 1.7 mg/dL) when feeding LAC compared with CON. Liver lipid content was decreased (8.6. vs. 14.7 ± 1.5% of wet weight) in cows fed LAC relative to those fed CON, whereas liver glycogen was not affected by dietary treatments. Feeding lactose to transition dairy cows increased the proportion of butyrate in the rumen and β-hydroxybutyrate in plasma and decreased liver lipid but did not affect lactation performance.     

Browning,Starch Gelatinization,Water Sorption,Glass Transition,and Caking Properties of Freeze-dried Maca ( Lepidium meyenii Walpers) Powders

The browning, gelatinization of starch, water sorption, glass transition, and caking properties of freeze-dried maca ( Lepidium meyenii Walpers) powders were investigated and compared with a commercial maca powder. The freeze-dried maca powders had lower optical density (browning) and higher enthalpy change for starch gelatinization than the commercial maca. This resulted from a difference in thermal history. The equilibrium water contents of the freeze-dried maca powders were higher than those of commercial maca at each water activity ( a _w ) because of differences in amorphous part. The glass transition temperature ( T _g ) was evaluated by differential scanning calorimetry. There was a negligible difference in the anhydrous T _g (79.5–80.2 ºC) among the samples. The T _g -depression of freeze-dried maca powders induced by water sorption was more gradual than that of the commercial maca due to a difference in water insoluble material content. From the results, critical water activity ( a _wc ) was determined as the a _w at which T _g becomes 25 ºC. There was negligible caking below a _w = 0.328. At higher a _w , the degree of caking remarkably increased with a large variation depending on the samples. The degree of caking could be described uniformly as a function of a _w / a _wc . From these results, we propose an empirical approach to predict the caking of maca powders.     

赖氨酸硫酸盐结块问题探析

论述了赖氨酸硫酸盐生产及存储过程中结块产生的原因及其影响因素,并简述了缓解赖氨酸硫酸盐结块的有效方法.     

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.     

Identification of lactose ureide, a urea derivative of lactose, in milk and milk products

With the widespread consumption of milk, the complete characterization of the constituents of milk and milk products is important in terms of functionality and safety. In this study, a novel nonreducing carbohydrate was separated from powdered skim milk and was identified using electron spray ionization-mass spectrometry (m/z 385.1[M + H⁺]), ¹H, ¹³C, ¹H¹H-correlation spectroscopy, and heteronuclear single quantum-nuclear magnetic resonance spectra. The carbohydrate was identified as a lactose derivative of urea, N-carbamoyl-o-β-d-galactopyranosyl-(1–4)-d-glucopyranosylamine (lactose ureide, LU). For the HPLC analysis of LU in milk and milk products, benzoylated LU, hepta-o-benzoyl lactose ureide (melting point 137–139 °C; m/z 1,113 [M + H⁺]; wavelength of maximum absorption, λ_max, 229 nm; molar extinction coefficient, ε, 8.1037 × 10⁷), was used as a standard. The crude nonreducing carbohydrate fraction from raw milk, thermally processed milk, and milk products such as powdered milks were directly benzoylated and subjected to HPLC analysis using an octadecylsilyl column to determine the quantity of LU. The content of LU in 10% solutions of powdered skim milk and powdered infant formula (5.0 ± 1.1 and 4.9 ± 1.5 mg/L, respectively) were almost 3-fold higher than that of UHT milk (1.6 ± 0.5 mg/L) and higher than that of low-temperature, long-time-processed (pasteurized at 65 °C for 30 min) milk (1.2 ± 0.3 mg/L) and the fresh raw milk sample (0.3 ± 0.1 mg/L). A time-course of the LU content in raw milk during heating at 110 °C revealed that LU increased with time. From these results, it is likely that LU is formed by the Maillard-type reaction between the lactose and urea in milk and milk products. Because the concentration of LU in milk increased with the degree of processing heat treatment, it could serve as an indicator of the thermal deterioration of milk. Although it is known that the human intestine is unable to digest LU, the gastrointestinal bacteria in human subjects are able to digest and utilize urea nitrogen in formation of essential amino acids that are available to the host human. These findings suggest that LU in milk might have a functional role in human health.     

Recovery of lactose from simulated delactosed whey permeate by a low-temperature crystallization process

Delactosed whey permeate is the mother liquor/by-product of lactose manufacture, but it still contains around 20 wt% lactose. The high mineral content, stickiness, and hygroscopic behavior prevent further recovery of lactose in the manufacturing process. Therefore, its use is currently limited to low-value applications such as cattle feed, and more often it is seen as waste. This study investigates a new separation technique operating at sub-zero conditions. At low temperature, precipitation of calcium phosphate is expected to be reduced and the lower solubility at sub-zero temperature makes it possible to recover a large portion of the lactose. We found that lactose could be crystallized at sub-zero conditions. The crystals had a tomahawk morphology and an average size of 23 and 31 µm. In the first 24 h, the amount of calcium phosphate precipitated was limited, whereas the lactose concentration was already close to saturation. The overall rate of crystallization was increased compared with the crystals recovered from a pure lactose solution. Mutarotation was rate limiting in the pure system but it did not limit the crystallization of lactose from delactosed whey permeate. This resulted in faster crystallization; after 24 h the yield was 85%.     

微生物对储藏稻谷结块及品质影响的研究

本实验研究了微生物对稻谷结块的影响,并系统地测定和分析了稻谷结块前后的出糙率、不完善粒率、整精米率、垩白粒率、直链淀粉含量、α-淀粉酶、过氧化物酶、脂肪酶、游离脂肪酸值及糊化特性等品质指标的变化。研究发现,黑曲霉、黄曲霉以及产黄青霉最易导致稻谷结块,此外结块稻谷的出糙率、整精米粒率较低,并且不完善粒率明显增加,其中结块稻谷的整精米率55%,不完善粒率5%,已无法达到国家三级粳稻谷的要求。并且稻谷中淀粉的结构发生了一定的变化,使得淀粉抗剪切能力下降,淀粉粒更易破裂,而所制得的米饭,其硬度大,黏性小,整体品质较差。此外在X射线衍射及扫描电子显微镜的测试中发现结块稻谷的淀粉结晶度增大,并且微观结构存在团聚现象,由此推测在微观层面稻谷内淀粉结构的变化是引起稻谷宏观品质变化的重要因素。本实验研究了不同优势微生物对稻谷结块的影响,系统并全面地分析稻谷结块前后的品质变化,为我国粮食安全储藏提供理论依据,科学指导储粮实践。     

无水柠檬酸结块行为研究

研究了不同空气相对湿度、温度、晶体粒径以及添加剂（甘油）对无水柠檬酸晶体结块行为的影响。结果表明,空气相对湿度、温度以及添加剂（甘油）是主要影响因素。35℃下低于临界相对湿度（约75%）或温度高于晶型转换温度（约36.6℃）时储存晶体不会结块。此外,添加1%（wt）的甘油也能阻止结块现象的发生。通过运用光学显微镜、扫描电镜（SEM）及差示扫描量热仪（DSC）对结块产品进行分析认为,无水柠檬酸的结块机理为无水酸向一水酸的晶型转化过程中,水分的吸收和挥发造成了晶体的溶解-重结晶并形成晶桥。      

Retention of Diacetyl in Milk during Spray-Drying and Storage

Spray-drying of milk in a Leaflash dryer was studied in relation to volatile aroma loss in drying and during storage of the powders. Diacetyl was used as the volatile model, and the contribution of the various milk constituents to retention was determined. Proteins retain more diacetyl than does lactose or fat. Conditions leading to a powder with more amorphous lactose result in higher diacetyl loss during drying. The rate of diacetyl loss during storage depended on relative humidity and on the T — T_g parameter and was strongly enhanced by crystallization of amorphous lactose.     

食品粉末颗粒间的相互作用及结块行为的研究概述

粉体结块现象是食品工业中普遍存在的实际问题。本文针对食品粉体结块现象进行了综述,阐述了粉末颗粒间的相互作用,介绍了食品粉末结块的测试方法,分析了食品粉末结块动力学行为与结块控制方法,提出食品粉末结块研究中需要跟踪粉末颗粒间桥联的演变过程,并总结传热传质模型对食品粉末结块行为的重要作用,旨在为食品粉末结块的有效控制提供参考。