甘蔗糖蜜羰氨反应制备香料的技术研究
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摘要
本课题探讨了以廉价的甘蔗糖蜜为原料,通过羰氨反应制备香料的工艺技术。研究了不同预处理工艺对糖蜜制备香料的影响,并采用气质色谱联用技术(GC/MS)分析香料成品的挥发性风味成分。在此基础上,进行了不同方法强化糖蜜制香的工艺研究。
1.通过单因素和正交实验,确定甘蔗糖蜜预处理工艺条件如下:原糖蜜与蒸馏水按1:5稀释;采用磷酸辅助絮凝剂法进行絮凝澄清:添加0.025%磷酸,石灰水调节pH值至中性,加0.0005%聚丙烯酰胺,85℃恒温水浴中保温10min进行二次絮凝,离心,取上清液;硫酸法酸解糖蜜:酸解温度100℃、pH值2及酸解时间90min;再经电压30V,流速70L/hr的电渗析工艺脱盐。去除了糖蜜中大部分杂质,提高了糖蜜的纯度,并采用GC/MS分析预处理前后糖蜜成分的变化。
2.采用硅胶柱层析法验证了以糖蜜为原料羰氨反应制备香料的可行性。探究了不同预处理工艺对糖蜜羰氨制香的影响,羰氨反应后,四种糖蜜反应体系RMS、FMS、CMS和DMS中pH值均有下降,吸光度、色值和金属还原力均有上升,其中FMS变化幅度最大。采用GC/MS分析羰氨产物RMP、FMP、CMP和DMP的挥发性物质成分,发现有醛酮类、醇酸类、氮杂环类(如吡嗪,呋喃等)、酚类和酯类以及烷烃类化合物,但各类化合物所占百分含量各不相同,RMP和CMP均以酚类化合物含量最高,FMP中酯类化合物含量最高,而DMP以醇酸类化合物含量最高。
3.研究了超高静压、超声波、微波三种辅助方法对糖蜜羰氨制香的影响,三种方法羰氨制备的产物分别是PMP、UMP和MMP,经GC/MS分析,发现PMP和MMP中皆以吡嗪类化合物为主,而UMP中酯类化合物所占比例较大。同样反应条件下制备的UMP与GGP相比,GGP以吡嗪类化合物为主,占总风味产物的56.26%,酯类化合物次之;而UMP中吡嗪类等产物所占比例均衡,酯类化合物占比最大,可以采用廉价的糖蜜替代纯葡萄糖进行羰氨反应制备香料。
4.采用响应面和嵴岭分析方法对超高静压辅助糖蜜羰氨制香的工艺进行优化,得出PMP最佳制备条件:反应压力400MPa,反应体系初始pH值11,糖氨比(糖蜜中还原糖与氨基酸摩尔比)1:1;该工艺条件经实验验证后,PMP实际的金属还原力在700nm下测定的吸光度:1.915±0.009,与预测值2.049基本一致。且优化条件下制备的PMP在饼干和肉酱中的应用效果良好,产品中带有糖蜜特有的风味。
In this paper, sugarcane molasses was taken as a raw material to produce flavor according to Maillard Reaction. The effect of pretreatment on the flavor making from molasses was comprehensively studied, and GC/MS was applied to analyse the volatile of flavor. In addition, the techniques of making flavor from molasses by different methods were put into the research.
1. Single factor Experiment and Orthogonal Experiment were applied to study the pretreatment of molasses. The results were as followed: molasses was diluted in 6 times. H3PO4 and PAM co-flocculation was adopted to clarify molasses in this way: 0.025% H3PO4 was added, adjusting pH to 7 by lime, mixing 0.0005% PAM, floccing in 85℃water-bath for 10min, centrifuging, and save supernatant liquid. Then, acidolysis molasses into reducing sugar on the condition of pH 2 and 100℃water-bath for 90min. Finally, electroosmosis was used on 30V, 70L/hr to desalt molasses, then, the changes of molasses component after pretreatment were analysed by GC/MS.
2. Silicagel column chromatography was adopted to verify the feasibility of making flavor from molasses, and the influence of pretreatment on flavor prepareation technology was investigated thoroughly. After Maillard reaction, pH of RMS, FMS, CMS and DMS were descended, while the absorbance, color, and reducing power were increased, especially in FMS. GC/MS was used to analyse the volatile of RMP, FMP, CMP and DMP. The results showed that they all contained Carbonyls, Alcohol, Nitrogen heterocyclic ring, phenols, esters and alkane, the biggest difference was the percentage of composition. Phenols were at most in RMP and CMP, and esters were maximum amount in FMP, while Alcohol compounds were the most part of DMP.
3. The influence of Ultra-high Hydrostatic Pressure, Ultrasound Wave, and Microwave on flavor prepareation technology was researched. Under the condition of Ultra-high Hydrostatic Pressure and Microwave, pyrazine was the main component of PMP and MMP, while Ultrasound Wave promoted the generation of esters better, although there were also some pyrazines produced in UMP. Compared UMP with GGP preparing under the same condition, pyrazine was most in GGP, accounting for 56.26%, and esters took second place. In UMP, there were carbonyls and phenols, more than just pyrazine and ester, that’s mean, the cheap molasses could replace glucose to make flavor according Maillard.
4. Finally, response surface experiment and SAS analysis software were employed to optimize the technology of making flavor from molasses under Ultra-high Hydrostatic Pressure. The optimum condition of producing PMP was as follows: reaction pressure was 400 MPa, pH of the initial system was 11 and Sugar: Amino acid in molasses was 1:1. The optimum condition was tested through experiment, which showed the reducing power of the Maillard products from molasses on 700nm was 1.915±0.009, which is in line with the predicted value of 2.049. PMP produced under the optimum condition was applied well in cookies and meat paste which were full of the special flavor from molasses.
1.通过单因素和正交实验,确定甘蔗糖蜜预处理工艺条件如下:原糖蜜与蒸馏水按1:5稀释;采用磷酸辅助絮凝剂法进行絮凝澄清:添加0.025%磷酸,石灰水调节pH值至中性,加0.0005%聚丙烯酰胺,85℃恒温水浴中保温10min进行二次絮凝,离心,取上清液;硫酸法酸解糖蜜:酸解温度100℃、pH值2及酸解时间90min;再经电压30V,流速70L/hr的电渗析工艺脱盐。去除了糖蜜中大部分杂质,提高了糖蜜的纯度,并采用GC/MS分析预处理前后糖蜜成分的变化。
2.采用硅胶柱层析法验证了以糖蜜为原料羰氨反应制备香料的可行性。探究了不同预处理工艺对糖蜜羰氨制香的影响,羰氨反应后,四种糖蜜反应体系RMS、FMS、CMS和DMS中pH值均有下降,吸光度、色值和金属还原力均有上升,其中FMS变化幅度最大。采用GC/MS分析羰氨产物RMP、FMP、CMP和DMP的挥发性物质成分,发现有醛酮类、醇酸类、氮杂环类(如吡嗪,呋喃等)、酚类和酯类以及烷烃类化合物,但各类化合物所占百分含量各不相同,RMP和CMP均以酚类化合物含量最高,FMP中酯类化合物含量最高,而DMP以醇酸类化合物含量最高。
3.研究了超高静压、超声波、微波三种辅助方法对糖蜜羰氨制香的影响,三种方法羰氨制备的产物分别是PMP、UMP和MMP,经GC/MS分析,发现PMP和MMP中皆以吡嗪类化合物为主,而UMP中酯类化合物所占比例较大。同样反应条件下制备的UMP与GGP相比,GGP以吡嗪类化合物为主,占总风味产物的56.26%,酯类化合物次之;而UMP中吡嗪类等产物所占比例均衡,酯类化合物占比最大,可以采用廉价的糖蜜替代纯葡萄糖进行羰氨反应制备香料。
4.采用响应面和嵴岭分析方法对超高静压辅助糖蜜羰氨制香的工艺进行优化,得出PMP最佳制备条件:反应压力400MPa,反应体系初始pH值11,糖氨比(糖蜜中还原糖与氨基酸摩尔比)1:1;该工艺条件经实验验证后,PMP实际的金属还原力在700nm下测定的吸光度:1.915±0.009,与预测值2.049基本一致。且优化条件下制备的PMP在饼干和肉酱中的应用效果良好,产品中带有糖蜜特有的风味。
In this paper, sugarcane molasses was taken as a raw material to produce flavor according to Maillard Reaction. The effect of pretreatment on the flavor making from molasses was comprehensively studied, and GC/MS was applied to analyse the volatile of flavor. In addition, the techniques of making flavor from molasses by different methods were put into the research.
1. Single factor Experiment and Orthogonal Experiment were applied to study the pretreatment of molasses. The results were as followed: molasses was diluted in 6 times. H3PO4 and PAM co-flocculation was adopted to clarify molasses in this way: 0.025% H3PO4 was added, adjusting pH to 7 by lime, mixing 0.0005% PAM, floccing in 85℃water-bath for 10min, centrifuging, and save supernatant liquid. Then, acidolysis molasses into reducing sugar on the condition of pH 2 and 100℃water-bath for 90min. Finally, electroosmosis was used on 30V, 70L/hr to desalt molasses, then, the changes of molasses component after pretreatment were analysed by GC/MS.
2. Silicagel column chromatography was adopted to verify the feasibility of making flavor from molasses, and the influence of pretreatment on flavor prepareation technology was investigated thoroughly. After Maillard reaction, pH of RMS, FMS, CMS and DMS were descended, while the absorbance, color, and reducing power were increased, especially in FMS. GC/MS was used to analyse the volatile of RMP, FMP, CMP and DMP. The results showed that they all contained Carbonyls, Alcohol, Nitrogen heterocyclic ring, phenols, esters and alkane, the biggest difference was the percentage of composition. Phenols were at most in RMP and CMP, and esters were maximum amount in FMP, while Alcohol compounds were the most part of DMP.
3. The influence of Ultra-high Hydrostatic Pressure, Ultrasound Wave, and Microwave on flavor prepareation technology was researched. Under the condition of Ultra-high Hydrostatic Pressure and Microwave, pyrazine was the main component of PMP and MMP, while Ultrasound Wave promoted the generation of esters better, although there were also some pyrazines produced in UMP. Compared UMP with GGP preparing under the same condition, pyrazine was most in GGP, accounting for 56.26%, and esters took second place. In UMP, there were carbonyls and phenols, more than just pyrazine and ester, that’s mean, the cheap molasses could replace glucose to make flavor according Maillard.
4. Finally, response surface experiment and SAS analysis software were employed to optimize the technology of making flavor from molasses under Ultra-high Hydrostatic Pressure. The optimum condition of producing PMP was as follows: reaction pressure was 400 MPa, pH of the initial system was 11 and Sugar: Amino acid in molasses was 1:1. The optimum condition was tested through experiment, which showed the reducing power of the Maillard products from molasses on 700nm was 1.915±0.009, which is in line with the predicted value of 2.049. PMP produced under the optimum condition was applied well in cookies and meat paste which were full of the special flavor from molasses.
引文
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