液态乳中掺有复原乳的乳果糖检测方法

目的:比较乳果糖的3种紫外分光光度检测方法,优选出一较好的方法来检测液态乳中是否掺有复原乳。方法:以生乳、复原乳、掺有复原乳的巴氏杀菌乳和UHT灭菌乳为试样,分别采用Adhikari、蒽酮和Seliwanoff’s比色方法来检测生乳和复原乳的差别,选定一种较好的方法测定复原乳的掺入率。结果:用Seliwanoff’s比色法检测液态乳中乳果糖的含量,在生乳和巴氏杀菌乳中掺有15%的复原乳,UHT灭菌乳中掺有20%的复原乳。结论:乳果糖的Seliwanoff’s测定法可以快速检测液态乳中是否掺有复原乳。     

热处理对生鲜乳及复原乳蛋白质体外消化特性的影响

通过体外模拟消化的方法对不同热处理的牛乳样品进行检测,研究热处理对鲜牛乳及复原乳营养价值的影响。通过聚丙烯酰氨凝胶电泳、尺寸排阻高效液相色谱、扫描电镜及质谱分析等多种方法进行检测。结果表明:经过胃液消化后,牛乳中的部分蛋白被消化,其中酪蛋白消化最为明显,鲜牛乳中酪蛋白在胃液中的消化水平高于其他热处理样品;而经过肠液消化后,牛乳中蛋白消化完全,生成游离氨基酸及小肽。乳中蛋白质经消化主要生成分子质量低于1 500 Da的肽段,易于人体消化吸收。通过扫描电镜可以看出,热处理程度越大,乳蛋白变性,发生聚集现象,粒径增大,其中加热复原乳的粒径较其他乳制品大;通过质谱检测及高效液相色谱分析,热处理程度越大,蛋白质美拉德反应程度升高。     

采用双向电泳技术研究牛乳热加工后蛋白质组变化

采用双向电泳技术建立牛乳蛋白质组检测方法,研究不同热加工条件对牛乳主蛋白成分含量的影响,从而对不同热处理牛乳,包括鲜乳,巴氏乳,复原乳等进行鉴别。     

热处理对液态乳中乳清蛋白的影响研究进展

牛乳中的乳清蛋白主要包括β-乳球蛋白、α-乳白蛋白、牛血清白蛋白和免疫球蛋白。在牛乳加工过程中,热处理会使乳中乳清蛋白发生变性,影响了乳清蛋白的结构和活性,进而降低了牛乳的营养价值。本文对乳业发达国家液态乳的主要加工方式以及热处理过程对4种乳清蛋白的影响进行了综述。     

热处理对鲜牛乳和复原孔蛋白多态性的影响

利用三种模拟生产加热处理,来研究鲜牛乳和复原乳蛋白多态性变化.通过调控pH和加热温度,发现鲜牛乳和复原乳中α-乳白蛋白、β-乳球蛋白、非沉淀酪蛋白和蛋白胶束的粒径大小均变化差异显著.     

农业部发布巴氏杀菌乳和UHT灭菌乳中复原乳鉴定标准

农业部日前发布《巴氏杀菌乳和UHT灭菌乳中复原乳的鉴定》标准,为巴氏杀菌乳和UHT灭菌乳中复原乳成分的检测提供了科学依据。国务院办公厅《关于加强液态奶生产经营管理的通知》要求,完善液态奶标准并严格按标准组织生产凡在灭菌乳、酸牛乳等产品生产加工过程中使用复原乳的,不论数量多少,自今年10月15日起,生产企业必须在其产品包装上醒目标注“复原乳”。但目前我国的国家标准、行业标准中,还没有复原乳检测方法标准。为落实好国办《通知》精神,农业部在以往研究工作的基础上,组织专家组制定了《巴氏杀菌乳和UHT 灭菌乳中复原乳的鉴定》标准。     

温度与复原度对巴氏杀菌乳中糠氨酸含量影响的研究

采用农业部标准NY/T 939-2005中的方法对巴氏杀菌乳中的糠氨酸进行检测,测定不同杀菌温度及不同复原度条件下牛乳中的糠氨酸含量。对糠氨酸含量随温度和复原度的变化规律进行研究,得到不同复原度的复原乳在不同温度下的糠氨酸含量数据,并对数据进行分析处理,制定了不同温度下的糠氨酸与复原度的线性回归方程。研究结果可对复原乳进行的定性判别和定量检测,以避免对复原乳的误判。     

基于电子舌的掺假牛乳的快速检测

以掺假牛乳样品为检测对象,利用电子舌结合主成分分析法进行研究,旨在寻求一种能有效监控牛乳品质的快速检测方法.对几种常见的掺假(掺入水、食盐、蔗糖、尿素、大豆油)牛乳样品、复原乳以及纯牛乳样品进行检测和评价.试验结果表明:电子舌可以很好地区分纯牛乳和掺入不同物质的牛乳样品,纯牛乳、纯鲜牛乳、复原乳及其混合乳样品得到有效辨识,同时各种掺假牛乳样品随掺入物质的比例在主成分得分图中呈规律性分布.电子舌可用于掺假牛乳的快速检测.在建立典型标准样品数据库的前提下电子舌可有效监控牛乳品质,其在乳制品的质量控制及评价中具有较大的应用潜力.     

关于复原乳标识标注有关问题的通知

各省、自治区、直辖市质量技术监督局:《国务院办公厅关于加强液态奶生产经营管理的通知》(以下简称《通知》)要求:在巴氏杀菌乳生产中不允许添加复原乳,大力提倡和鼓励在灭菌乳生产中全部使用生鲜乳。自2005年10月15日起,用乳粉或在生鲜乳中添加部分乳粉生产的酸牛乳、灭菌乳必须标注“复原乳”,10月15日前生产但未标注"复原乳"的奶制品允许销售至2006年1月15日。为落实《通知》精神,规范复原乳标识标注,现就有关问题通知如下:一、使用复原乳生产加工液体乳标签必须标识的内容对于用乳粉或在生鲜乳中添加部分乳粉生产的酸牛乳、灭菌乳,其产…     

不同热处理液态牛乳产品中主要活性蛋白质量浓度差异研究

为了建立RP-HPLC方法快速准确测定不同热处理方式的市售液态牛乳中主要活性蛋白包括α-乳白蛋白（α-La）和β-乳球蛋白（β-Lg）的质量浓度,建立了测定活性乳蛋白所使用的RP-HPLC法,该法具有良好的稳定性（RSD<8%）和较高的回收率（>95%）。测定结果表明,与原料乳相比,经过高温处理（常温存放）的液态乳中的活性α-La和β-Lg显著偏低（<0.16 g/L）;而经巴氏杀菌后低温存放（2～6℃）的液态乳样品中活性乳蛋白可得到很好地保持,部分灭菌后低温存放的样品中活性蛋白损失较大。本研究旨为优化液态乳热处理工艺和规范乳企业对于液态乳的工业生产提供借鉴,为消费者对液态乳制品的选择提供指导。     

Effects of heating temperatures and addition of reconstituted milk on the heat indicators in milk

The objective of the present study was to evaluate the effect of heating temperatures and reconstituted milk on heat treatment indicators in milk by comparing the heat damage between raw milk and raw milk plus reconstituted milk (composite milk). The contents of lactulose, furosine, beta-lactoglobulin, and lactoperoxidase were determined after the heat indicators were heated to 65 to 115 °C for 15 s both in raw milk and composite milk. In the raw milk, the lactulose and furosine contents increased with increased heating temperature, while the beta-lactoglobulin content and lactoperoxidase activity decreased. The lactulose and furosine contents were increased after the addition of reconstituted milk. The reconstituted milk also significantly (P < 0.05) reduced the concentration of beta-lactoglobulin in the milk. Both heat treatment and an addition of reconstituted milk decreased the lactoperoxidase activity significantly (P < 0.05), and the lactoperoxidase activity was undetectable at 85 °C. The ratios of lactulose to furosine in pasteurized milk were higher than that in composite pasteurized milk. It is concluded that lactulose, furosine, and beta-lactoglobulin are suitable indicators of high heat pasteurization or raw milk, while lactoperoxidase may be used in monitoring mild heat pasteurization. Practical Application: Adequate heat treatment is necessary to destroy the microbes in raw milk. However, excessive heat treatment can result in inactivation of active compounds or loss of nutrients. The present study showed that the concentrations of lactulose, furosine, beta-lactoglobulin, and the activity of lactoperoxidase are sensitive to processing temperature and can serve as indicators of milk pasteurization.     

Effect of the protein, citrate and phosphate content of milk on formation of lactulose during heat treatment

Milk ultrafiltrate and milks of varying protein, citrate and phosphate concentrations were heated in sealed containers. Protein was found not to be involved in the mechanism of formation of lactulose, but increasing the protein content of milk reduced the concentration of lactulose after heating. This was considered to be due to increased condensation of lactose and lactulose with amino groups of the protein. Less lactulose was formed in milk ultrafiltrate than in skimmed milk accorded the same heat treatment, which was attributed to the buffering capacity of the milk protein in skimmed milk. Activation energies for lactulose formation in skimmed milk and in ultrafiltrate were 128 and 131 kJ/mol respectively. Citrate and phosphate catalysed the formation of lactulose. It is proposed that the formation of free lactulose in heated milk and ultrafiltrate proceeds exclusively by the Lobry de Bruyn-Alberda van Ekenstein transformation with the naturally occurring phosphate and citrate acting as base catalysts.     

Lactulose as a food ingredient

Lactulose is a synthetic ketose disaccharide that can be obtained from lactose by different methods of synthesis. Chemical methods are based on the isomerization of lactose in the presence of basic catalysts and enzymatic methods using lactose as a galactose donor and fructose as an acceptor. The prebiotic properties of lactulose have been known for more than 50 years and numerous studies have confirmed several health benefits of lactulose as a food ingredient, including selective stimulation of intestinal flora, laxative effect and improvement of calcium absorption. Its use in fermented milk manufacture may reduce the incubation period and favour the growth of bifidobacteria. The synthesis of lactulose‐derived oligosaccharides may provide a new group of prebiotics with properties complementary to those of native lactulose. Copyright © 2009 Society of Chemical Industry     

Effects of overprocessing on heat damage of UHT milk

Formation of lactulose, furosine, galactosyl-|*beta*|-pyranone and lysinoalanine was studied in UHT milk samples produced by either direct or indirect heating on industrial plants and by indirect heating on a pilot plant. In particular, the effects of severe sterilization conditions, different proportions of milk recirculation, and storage of the finished product (23 °C for up to 90 days) have been investigated on the levels of the above molecules in UHT milk. An extensive increase of the values of all the indicators occurred when severe heat process was applied, but no direct relation was found between their levels and the nominal time–temperature conditions. Lactulose and furosine levels confirmed to be strictly correlated in UHT milk. In case of overheating or high proportion (60%) of milk recirculation, galactosyl-|*beta*|-pyranone formation was strongly enhanced, proving that also the advanced Maillard reaction takes place extensively, which is not detected by furosine value. Formation of lysinoalanine in UHT drinking milk on storage was pointed out for the first time. Lysinoalanine proved to be the most sensitive index of storage conditions among the four parameters studied. Data suggest that a realistic defence of UHT milk quality can be achieved only by fixing upper limits to heat damage parameters. Besides avoiding unjustified milk overheating, this approach may allow manipulations, like reprocessing expired milk, to be pointed out.     

复原乳鉴别指标探讨

选择适宜的鉴别指标,确定并完善复原乳的鉴定方法,不但可为质量监督检验机构的检测和监督工作提供技术支持．而且可有效保护消费者的利益。可以通过检测牛奶在长时间贮藏过程中产生的荧光物质．或检测牛奶中脂肪酸组成分的变化来鉴别鲜奶与复原乳,但难以排除某些干扰因素的影响。近年来复原乳鉴定指标的研究热点主要集中在奶制品经热处理后其中的热损害产物。有两种化学反应产物可用来评价：（1）降解产物：热不稳定组分的降解、变性、失活,如乳清蛋白或酶;（2）新形成物质：如乳果糖或美拉德反应的产物。目前国际上通常用糠氨酸和乳果糖作为评估热处理和贮存对奶制品质量影响的指标。然而各指标也不可避免的存在一定的局限性,因此可能需要不止一个指标来进行综合评价。     

Heat stability of reconstituted, protein-standardized skim milk powders

We determined the effects of standardization material, protein content, and pH on the heat stability of reconstituted milk made from low-heat (LH) and medium-heat (MH) nonfat dry milk (NDM). Low-heat and MH NDM were standardized downward from 35.5% to 34, 32, and 30% protein by adding either edible lactose powder (ELP) or permeate powder (PP) from skim milk ultrafiltration. These powders were called standardized skim milk powders (SSMP). The LH and MH NDM and SSMP were reconstituted to 9% total solids. Furthermore, subsamples of reconstituted NDM and SSMP samples were set aside to measure heat stability at native (unadjusted) pH, and the rest were adjusted to pH 6.3 to 7.0. Heat stability is defined as heat coagulation time at 140°C of the reconstituted LH or MH NDM and SSMP samples. The entire experiment was replicated 3 times at unadjusted pH values and 2 times at adjusted pH values. At an unadjusted pH, powder type, standardization material, and protein content influenced the heat stability of the samples. Heat stability for reconstituted LH NDM and SSMP was higher than reconstituted MH NDM and SSMP. Generally, decreased heat stability was observed in reconstituted LH or MH SSMP as protein content was decreased by standardization. However, adding ELP to MH SSMP did not significantly change its heat stability. When pH was adjusted to values between 6.3 and 7.0, powder type, standardization material, and pH had a significant effect on heat stability, whereas protein content did not. Maximum heat stability was noted at pH 6.7 for both reconstituted LH NDM and SSMP samples, and at pH 6.6 for both reconstituted MH NDM and SSMP samples. Furthermore, for samples with adjusted pH, higher heat stability was observed for reconstituted LH SSMP containing PP compared with reconstituted milk from LH SSMP containing ELP. However, no statistical difference was observed in the heat stability of reconstituted milk from MH NDM and MH SSMP samples. We conclude that powder type (LH or MH) and effect of standardization material (ELP or PP) can help explain differences in heat stability. The difference in the heat stability of powder type may be associated with the difference in the pH of maximum heat stability and compositional differences in the standardization material (ELP or PP).     

HPLC Determination of Lactulose in Heat Treated Milk

Lactulose (4-O-β-d-galactopyranosyl-d-fructose), formed from lactose (4-O-β-d-galactopyranosyl-d-glucose) by the Lobry de Bruyn–Alberda van Ekenstein rearrangement during severe heat treatments, is considered a useful indicator of heat-induced modifications in milk. Its chromatographic determination in milk is particularly troublesome due to the concomitant presence of a lactose amount two orders of magnitude larger than the lactulose amount and to a similar retention time of the two compounds. In this work, four HPLC methods have been compared with the aim to develop a more accurate analytical procedure to determine lactulose in milk, together with lactose. The developed method is based on a Carrez precipitation followed by a HPLC separation on two in-series amino-based columns, using CH₃CN:H₂O 75:25 (v:v) as the mobile phase at 1 ml/min flow rate and a refractive index as the detector. The linearity test for the quantitation of lactulose has been carried out over the range 0.060–1.006 mg/ml, the limit of detection, is 0.013 mg/ml (256 ng injected) and the limit of quantitation is 0.028 mg/ml (556 ng injected). The proposed method, simple, cheap and time-saving, allows an accurate lactulose–lactose separation, with conventional HPLC equipment.     

Biocatalytic Approaches Using Lactulose: End Product Compared with Substrate

Lactulose is a lactose‐based carbohydrate with well‐known prebiotic effect and recognized medical applications. Currently, the commercially available lactulose is chemically synthesized. Nevertheless, the process leads to low yields and high levels of by‐products. Alternatively, lactulose can be produced by enzymatic synthesis, which provides a cleaner production under mild conditions. Two different enzymatic routes were reported for lactulose production. Lactulose can be obtained through hydrolysis and transfer reactions catalyzed by a glycosidase. Alternatively, lactulose can be produced by direct isomerization of lactose to lactulose catalyzed by cellobiose‐2‐epimerase. An interesting characteristic of lactulose is also its capacity to act as substrate in additional enzymatic synthesis which leads to the formation of attractive compounds, such as lactulose‐based oligosaccharides and lactulose esters. Besides increasing the interest and potential of lactulose, these lactulose‐based compounds can also offer new and promising functionalities and applications. Herein, we review the enzymes involved in the synthesis of lactulose, as well as the reaction conditions and yields. The potential of different enzymes is discussed and it is shown that reaction conditions and composition of products depend on the type of enzyme and its microbial source. The conversion of lactulose into lactulose‐based compounds is also covered, describing in detail the biocatalysts involved, the reaction conditions used, and the potential of the final products obtained.     

Variation in the lactulose content of UHT milk during the running of a pilot and a commercial indirectly heated plant

The lactulose content of UHT milk was measured during the running of a pilot and a commercial indirectly heated UHT plant. The lactulose content of milk processed in the pilot plant was found to decrease as the pressure drop across the heated sections rose. The lactulose content of the milk from the commercial plant varied little and showed no trend during an entire production shift. There was no evidence that deposit in the plants accelerated the formation of lactulose.     

Use of different thermal indices to assess the quality of pasteurized milks

 Lactoperoxidase activity and lactulose, furosine and undenatured whey protein contents were determined in Spanish commercial milks labelled as pasteurized (group A) and high-temperature pasteurized (group B), in order to assess their quality. Three samples of group A and all of the samples of group B were lactoperoxidase negative. Most samples of group A had measurable amounts of lactulose, even though their concentrations of undenatured β-lactoglobulin were higher than 2600 mg/l. In general, samples of group B showed higher lactulose and furosine and lower undenatured whey protein contents. High levels of furosine and lactulose accompanied by high levels of undenatured β-lactoglobulin could indicate the addition of milk heated at high temperatures, whereas high levels of furosine and relatively low levels of lactulose may have been due to the presence of reconstituted milk powder.