牛乳加热及乳粉加工中热相关工艺对氧化风味的影响研究
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摘要
由于生鲜乳的供应存在地域、季节等因素的限制，乳粉的加工和使用一直受到人们的重视。无论乳粉被直接消费，还是复原后替代生鲜乳作为生产原料应用于食品中，都存在一定的缺陷。其中，乳粉加工及贮藏过程中发生的氧化风味劣变是限制其食用和应用的主要瓶颈。本课题的目的是研究加热处理以及乳粉加工中的热相关工艺，包括预热、浓缩、干燥对牛乳中氧化风味物质（OFC）的影响；分析牛乳体系中脂质氧化环境和风味前体的暴露情况，同时分析乳粉颗粒的形态和表面组成特性受加工工艺的影响情况，研究它们在加工环节和乳粉贮藏环节对氧化风味形成的作用及潜在机理。
首先，采用固相微萃取-气相色谱-质谱分析加热乳中的挥发性物质，发现OFC随加热强度的增加而增加，与原料乳相比，90℃超过2min加热可明显增加己醛含量（P<0.05），90℃、20min加热时己醛含量增加了2.70倍；在设定的加热强度内，建立了OFC和加热参数之间良好的回归关系：决定系数大于0.86。加热后牛乳体系的氧化环境发生改变，与原料乳相比，90℃、20min加热时，DPPH·清除率降低了23.15%，过氧化值（POV）增加了37.23%。对OFC前体（乳脂肪）受热破坏情况的研究发现：低强度加热不会导致脂肪球分布出现明显变化；同时，随着加热强度的增加乳脂肪球膜中的具有保护作用的XDH/XO和BTN蛋白逐步遭到破坏。
乳粉加工中热相关工艺对OFC形成的影响研究表明：与原料乳和加热乳相比，浓缩乳和乳粉中OFC显著增加，而浓缩乳中的OFC略高于乳粉。此外，也发现浓缩溜出液中OFC的浓度高于浓缩乳，这表明浓缩过程中发生风味物质损失的同时，也会发生严重的脂质氧化反应。对乳粉加工过程中牛乳氧化环境和风味前体暴露情况的研究表明，与原料乳相比，经过预热、浓缩及干燥处理后，牛乳体系的DPPH·清除率出现不同程度的降低，而POV呈现增加趋势；浓缩后牛乳脂肪球发生了聚集，浓缩乳的脂肪球d3,2显著增加（P<0.05）；加热或浓缩均可改变乳脂肪球膜中XDH/XO和BTN蛋白组成。通过分析指出乳粉加工工艺造成的牛乳体系中氧化环境和风味前体暴露情况的显著改变，是OFC显著增加的诱因和起点。
乳粉的颗粒特性与贮藏后氧化风味的形成密不可分。乳粉颗粒表面特性分析发现：仅干燥工艺显著影响乳粉表面游离脂肪含量（P<0.05）；乳粉贮藏后表面游离脂肪中油酸、亚油酸及总不饱和脂肪酸的含量降低不明显；X射线光电子能谱分析表明乳粉颗粒的表面组成与整体组成明显不同，并且显著受热相关工艺影响。另外，乳粉颗粒影像信息的量化统计得到乳粉颗粒大小的范围为33.24-53.60μm，静态等温吸附测定得到乳粉颗粒的孔隙率范围为1.73-17.09mm3/g，发现这些乳粉颗粒的形态特性会受到乳粉工艺的影响，即这些乳粉的表面特性是工艺可控的。
乳粉OFC浓度在贮藏中呈现增加趋势，同时发现不同乳粉加工工艺及参数对贮藏中OFC的形成产生不同的影响。乳粉贮藏后复原乳的总抗氧化能力基本完全耗尽，而POV出现大幅度增加。乳粉颗粒特性与贮藏中OFC浓度的相关性研究发现：乳粉颗粒的形态而非颗粒的表面组成是造成贮藏中乳粉OFC显著增加的主要影响因素。
对贮存中乳粉的自由基检测结果表明：在贮藏3月和6月乳粉中均发现自由基存在，该自由基以单峰形式存在，g值为2.0054，随着贮藏时间的延长，自由基强度增加。另外，乳粉氧化风味的控制研究表明，添加抗坏血酸可以有效降低曝光或避光贮藏乳粉中OFC的形成，并发现形成了新的自由基。
最后，乳粉复原乳在酸奶中的应用研究表明：乳粉复原乳酸奶中醛类、甲基酮类、烯醛类、烯酮类、呋喃、苯并噻唑等化合物均有检出，新生产的乳粉复原乳酸奶中这些化合物含量较低，同时发现加热强度影响酸奶发酵剂的风味物质代谢，这些发现将为乳粉在酸奶中的应用奠定理论基础。
Attention has been paid to the production and application of milk powder dueto geographical, seasonal and other factors that limit raw milk supply. There aresome flaws both in the direct consumption of milk powder and in the alternative ofraw milk used in food after recovery of milk powder. The formation of oxidizedflavor during the production and storage of milk powder was a bottleneck thatrestricted the consumption and application of milk powder. The purpose of thepresent study was to investigate the effect of the heat treatment of bovine milk andthe thermal-related processes, including pre-heat, concentration and spray drying,during the manufacture of milk powder on the oxidized flavor compounds (OFC); toevaluate the environment of lipid oxidation and the exposure of the OFC precursorin process of bovine milk; to analyze the effect of the processes on the morphologyand surface composition of milk powder particle; and to research their effects andpotential mechanism on the formation of OFC both in the process sectors and instorage link of milk powder.
Firstly, the solid phase microextraction-gas chromatography-mass spectrometrywas used to analyze the volatiles in different heated milk, the content of OFCincreased with increasing the intensity of heat treatment. Compared with the rawmilk, the heat treatment at90℃for more than2min significantly increased thecontent of hexanal (P<0.05), and the heat treatment of90℃for20min increased thecontent of hexanal by2.70times. The regression relationship between OFC andheating parameters were built: the correlation coefficient was greater than0.86. Theheat treatment changed the oxidative environment of bovine milk: the treatment of90℃for20min reduced DPPH· scavenging activity by23.15%and increasedperoxide value (POV) by37.23%compared with the raw milk. The research on thethermal destruction of OFC precursor (milk fat) found that the low intensity of heatdid not cause the significant changes in the distribution of fat globules. Meanwhile,in milk fat globule membrane, the contents of XDH/XO and BTN proteins whichhave protective effect on the milk fat gradually destructed with the increasingintensity of heat treatment.
The research on effect of the thermal-related processes during the production ofmilk powder on the formation of OFC showed that the contents of OFC in theconcentrated milk or in milk powder were higher than those in raw milk or in heatedmilk and that the concentrated milk had higher contents of OFC compared with the milk powder. Besides, a higher content of OFC in distillate even than that in itscorresponding concentrated milk was found, suggesting that the severe lipidoxidation happened during concentration of milk with the loss of flavor compounds.According to the study on oxidative environment and exposure status of flavorprecursors, bovine milk decreased its DPPH· scavenging activity and increased itsPOV after the pre-heat, concentration or spray drying; compared to unconcentratedmilk, the d3,2of concentrated milk significantly increased (P<0.05) due to theaggregation of milk fat globules; the composition of XDH/XO and BTN proteinschanged by the processes of pre-heat and concentration and thus affected theirprotective effects on milk fat. In conclusion, the changes in the oxidativeenvironment and exposure of flavor precursors caused by the processing of bovinewere the reason and starting point for the formation of OFC.
The particle characteristics of milk powder have a close effect on the formationof oxidized flavor during the storage. Based on the analysis of composition, only theprocess of drying significantly affected the surface free-fat content in milk powderparticles (P<0.05); the contents of oleic acid, linoleic acid and the total unsaturatedfatty acid in surface free-fat did not change significantly during the storage of milkpowder; the surface composition of particles that was affected by the thermal-relatedprocesses showed a difference from the composition of total milk powder. Inaddition, the sizes of milk powder particles ranged from33.24to53.60μm by thequantitative statistics of images. The porosity of milk powder ranged from1.73to17.09mm3/g by static nitrogen adsorption method. The effects of the thermal-relatedprocesses on these morphological characteristics of milk powder particles weredetermined, that is, the characteristics were under control by these processes.
Levels of OFC in reconstituted milk had the increased tendency. It was alsofound that the formation of OFC during storage of milk powder could be influencedby the thermal-related processes. Total anti-oxidative activity of reconstituted milkpowder after storage almost depleted and POV substantially increased. Based on thecharacteristics of milk powder particles and concentrations of OFC during storage,the morphology of milk powder particles rather than the surface composition wasthe main influencing factor in the formation of OFC during storage of milk powder.
A free radical was detected in stored milk powder. The radical was in the formof a single peak with a g value of2.0054. The intensity of free radical increased withincreasing the storage time. In addition, the study on the control of OFC displayedthat the addition of ascorbic acid resulted in milk powder with low contents of OFCwhether in light-exposed or light-protected storage, and with the formation of newfree radical.
Finally, the reconstituted milk powder was used in the production of yogurt. Inresults, aldehydes, methyl ketones, olefinic aldehydes, ketenes, furan andbenzothiazole were detected in the yogurt produced from reconstituted milk powder.However, the yogurt that was produced with the newly produced milk powder hadthe low contents of these compounds. It was also found that the flavor metabolismof cultures during the fermentation of yogurt could be influenced by heat intensityof bovine milk. These results could expand existing apprehension on the applicationof milk powder in the manufacture of yogurt.
首先，采用固相微萃取-气相色谱-质谱分析加热乳中的挥发性物质，发现OFC随加热强度的增加而增加，与原料乳相比，90℃超过2min加热可明显增加己醛含量（P<0.05），90℃、20min加热时己醛含量增加了2.70倍；在设定的加热强度内，建立了OFC和加热参数之间良好的回归关系：决定系数大于0.86。加热后牛乳体系的氧化环境发生改变，与原料乳相比，90℃、20min加热时，DPPH·清除率降低了23.15%，过氧化值（POV）增加了37.23%。对OFC前体（乳脂肪）受热破坏情况的研究发现：低强度加热不会导致脂肪球分布出现明显变化；同时，随着加热强度的增加乳脂肪球膜中的具有保护作用的XDH/XO和BTN蛋白逐步遭到破坏。
乳粉加工中热相关工艺对OFC形成的影响研究表明：与原料乳和加热乳相比，浓缩乳和乳粉中OFC显著增加，而浓缩乳中的OFC略高于乳粉。此外，也发现浓缩溜出液中OFC的浓度高于浓缩乳，这表明浓缩过程中发生风味物质损失的同时，也会发生严重的脂质氧化反应。对乳粉加工过程中牛乳氧化环境和风味前体暴露情况的研究表明，与原料乳相比，经过预热、浓缩及干燥处理后，牛乳体系的DPPH·清除率出现不同程度的降低，而POV呈现增加趋势；浓缩后牛乳脂肪球发生了聚集，浓缩乳的脂肪球d3,2显著增加（P<0.05）；加热或浓缩均可改变乳脂肪球膜中XDH/XO和BTN蛋白组成。通过分析指出乳粉加工工艺造成的牛乳体系中氧化环境和风味前体暴露情况的显著改变，是OFC显著增加的诱因和起点。
乳粉的颗粒特性与贮藏后氧化风味的形成密不可分。乳粉颗粒表面特性分析发现：仅干燥工艺显著影响乳粉表面游离脂肪含量（P<0.05）；乳粉贮藏后表面游离脂肪中油酸、亚油酸及总不饱和脂肪酸的含量降低不明显；X射线光电子能谱分析表明乳粉颗粒的表面组成与整体组成明显不同，并且显著受热相关工艺影响。另外，乳粉颗粒影像信息的量化统计得到乳粉颗粒大小的范围为33.24-53.60μm，静态等温吸附测定得到乳粉颗粒的孔隙率范围为1.73-17.09mm3/g，发现这些乳粉颗粒的形态特性会受到乳粉工艺的影响，即这些乳粉的表面特性是工艺可控的。
乳粉OFC浓度在贮藏中呈现增加趋势，同时发现不同乳粉加工工艺及参数对贮藏中OFC的形成产生不同的影响。乳粉贮藏后复原乳的总抗氧化能力基本完全耗尽，而POV出现大幅度增加。乳粉颗粒特性与贮藏中OFC浓度的相关性研究发现：乳粉颗粒的形态而非颗粒的表面组成是造成贮藏中乳粉OFC显著增加的主要影响因素。
对贮存中乳粉的自由基检测结果表明：在贮藏3月和6月乳粉中均发现自由基存在，该自由基以单峰形式存在，g值为2.0054，随着贮藏时间的延长，自由基强度增加。另外，乳粉氧化风味的控制研究表明，添加抗坏血酸可以有效降低曝光或避光贮藏乳粉中OFC的形成，并发现形成了新的自由基。
最后，乳粉复原乳在酸奶中的应用研究表明：乳粉复原乳酸奶中醛类、甲基酮类、烯醛类、烯酮类、呋喃、苯并噻唑等化合物均有检出，新生产的乳粉复原乳酸奶中这些化合物含量较低，同时发现加热强度影响酸奶发酵剂的风味物质代谢，这些发现将为乳粉在酸奶中的应用奠定理论基础。
Attention has been paid to the production and application of milk powder dueto geographical, seasonal and other factors that limit raw milk supply. There aresome flaws both in the direct consumption of milk powder and in the alternative ofraw milk used in food after recovery of milk powder. The formation of oxidizedflavor during the production and storage of milk powder was a bottleneck thatrestricted the consumption and application of milk powder. The purpose of thepresent study was to investigate the effect of the heat treatment of bovine milk andthe thermal-related processes, including pre-heat, concentration and spray drying,during the manufacture of milk powder on the oxidized flavor compounds (OFC); toevaluate the environment of lipid oxidation and the exposure of the OFC precursorin process of bovine milk; to analyze the effect of the processes on the morphologyand surface composition of milk powder particle; and to research their effects andpotential mechanism on the formation of OFC both in the process sectors and instorage link of milk powder.
Firstly, the solid phase microextraction-gas chromatography-mass spectrometrywas used to analyze the volatiles in different heated milk, the content of OFCincreased with increasing the intensity of heat treatment. Compared with the rawmilk, the heat treatment at90℃for more than2min significantly increased thecontent of hexanal (P<0.05), and the heat treatment of90℃for20min increased thecontent of hexanal by2.70times. The regression relationship between OFC andheating parameters were built: the correlation coefficient was greater than0.86. Theheat treatment changed the oxidative environment of bovine milk: the treatment of90℃for20min reduced DPPH· scavenging activity by23.15%and increasedperoxide value (POV) by37.23%compared with the raw milk. The research on thethermal destruction of OFC precursor (milk fat) found that the low intensity of heatdid not cause the significant changes in the distribution of fat globules. Meanwhile,in milk fat globule membrane, the contents of XDH/XO and BTN proteins whichhave protective effect on the milk fat gradually destructed with the increasingintensity of heat treatment.
The research on effect of the thermal-related processes during the production ofmilk powder on the formation of OFC showed that the contents of OFC in theconcentrated milk or in milk powder were higher than those in raw milk or in heatedmilk and that the concentrated milk had higher contents of OFC compared with the milk powder. Besides, a higher content of OFC in distillate even than that in itscorresponding concentrated milk was found, suggesting that the severe lipidoxidation happened during concentration of milk with the loss of flavor compounds.According to the study on oxidative environment and exposure status of flavorprecursors, bovine milk decreased its DPPH· scavenging activity and increased itsPOV after the pre-heat, concentration or spray drying; compared to unconcentratedmilk, the d3,2of concentrated milk significantly increased (P<0.05) due to theaggregation of milk fat globules; the composition of XDH/XO and BTN proteinschanged by the processes of pre-heat and concentration and thus affected theirprotective effects on milk fat. In conclusion, the changes in the oxidativeenvironment and exposure of flavor precursors caused by the processing of bovinewere the reason and starting point for the formation of OFC.
The particle characteristics of milk powder have a close effect on the formationof oxidized flavor during the storage. Based on the analysis of composition, only theprocess of drying significantly affected the surface free-fat content in milk powderparticles (P<0.05); the contents of oleic acid, linoleic acid and the total unsaturatedfatty acid in surface free-fat did not change significantly during the storage of milkpowder; the surface composition of particles that was affected by the thermal-relatedprocesses showed a difference from the composition of total milk powder. Inaddition, the sizes of milk powder particles ranged from33.24to53.60μm by thequantitative statistics of images. The porosity of milk powder ranged from1.73to17.09mm3/g by static nitrogen adsorption method. The effects of the thermal-relatedprocesses on these morphological characteristics of milk powder particles weredetermined, that is, the characteristics were under control by these processes.
Levels of OFC in reconstituted milk had the increased tendency. It was alsofound that the formation of OFC during storage of milk powder could be influencedby the thermal-related processes. Total anti-oxidative activity of reconstituted milkpowder after storage almost depleted and POV substantially increased. Based on thecharacteristics of milk powder particles and concentrations of OFC during storage,the morphology of milk powder particles rather than the surface composition wasthe main influencing factor in the formation of OFC during storage of milk powder.
A free radical was detected in stored milk powder. The radical was in the formof a single peak with a g value of2.0054. The intensity of free radical increased withincreasing the storage time. In addition, the study on the control of OFC displayedthat the addition of ascorbic acid resulted in milk powder with low contents of OFCwhether in light-exposed or light-protected storage, and with the formation of newfree radical.
Finally, the reconstituted milk powder was used in the production of yogurt. Inresults, aldehydes, methyl ketones, olefinic aldehydes, ketenes, furan andbenzothiazole were detected in the yogurt produced from reconstituted milk powder.However, the yogurt that was produced with the newly produced milk powder hadthe low contents of these compounds. It was also found that the flavor metabolismof cultures during the fermentation of yogurt could be influenced by heat intensityof bovine milk. These results could expand existing apprehension on the applicationof milk powder in the manufacture of yogurt.
引文
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