水分散型番茄红素微乳的制备
摘要
番茄红素是脂溶性类胡萝卜素,具有很强的疏水性,在水及水基食品中的溶解度非常低,这严重限制了番茄红素在食品加工中的使用范围及作用效果,所以开发可在水基食品中使用的水分散型番茄红素产品具有重要意义。本文对水分散型番茄红素微乳的制备,微乳中番茄红素结构变化,微乳贮藏稳定性及其应用进行了系统研究。主要研究内容包括:
通过考察番茄红素在不同种类食用油、乳化剂、助乳化剂中的溶解情况,筛选出油相、乳化剂、助乳化剂的种类并确定Km值和配制温度范围;以乳化体系的稳定性为评价指标,采用正交实验对微乳的配方进行优化,确定番茄红素微乳体系的最优组合如下:选用中链甘油三酸酯为番茄红素的携带油脂,选用吐温40为乳化剂,选用乙醇为助乳化剂,确定番茄红素与中链甘油三酸酯的比例为1:3,表面活性剂和助表面活性剂的比例为吐温40:乙醇=11:6;确定微乳中油相、乳化剂混合物、水的质量比为1:5:8。该工艺下制备出含番茄红素微乳中番茄红素的含量可达4 mg/mL,粒径检测结果表明,微乳中番茄红素颗粒的Z-Ave粒径为14.34 nm。
依据现有的番茄红素异构体鉴定方法,分析微乳形成前后体系内番茄红素的结构变化。通过紫外-可见分光光度计全波长扫描,HPLC检测均显示微乳中有异构体产生; LC-MS分析证实在微乳化过程中产生的异构体主要是9-Z和13-Z。构型组成分析结果表明,处理前番茄红素以全反式为主,顺式构型和全反式构型所占比例分别是7.33%和92.67%;经过微乳化处理后,番茄红素中顺式构型所占比例为55.5%,全反式构型所占比例为44.5%。
通过分析发现,添加抗氧化剂可降低水分散型番茄红素微乳中番茄红素降解速率。通过考察不同种抗氧化剂抗氧化性以及对水分散型番茄红素微乳的影响,确定抗氧化剂的种类及用量为0.1 g/kg的L-抗坏血酰棕榈酸酯。
通过对水分散型番茄红素微乳在不同温度,避光/日光,有氧/驱氧条件下存放过程中番茄红素保留率变化的研究发现,在4℃、25℃、37℃下贮藏60天后,微乳中番茄红素的含量分别为:70.38%、62.66%、46.16%;在避光和日光条件下贮藏60天,微乳中番茄红素的含量分别为:62.66%、49.81%;在有氧、驱氧条件下贮藏60天,微乳中番茄红素的含量分别为:48.76%、82.26%;在避光条件下,将驱氧的水分散型番茄红素微乳分别贮藏于4℃和25℃环境中,4℃贮藏30天时保留率仍维持在90%以上,贮藏60天时,保留率为84.9%。在25℃贮藏60天,保留率为79.86%,由此得出最佳贮藏条件为:将水分散型番茄红素微乳在4℃避光驱氧保存。通过离心实验观察产品的质构稳定性,以沉积高度比w值为评价指标,可知当水分散型番茄红素微乳贮藏至10天、20天、60天时,w值分别为:0、3.3%、6%,证明微乳在一定时间内质构均一稳定。
将所制备的水分散型番茄红素微乳应用到饮料方面,配制出一种具有保健功能的新型饮料,其中番茄红素含量为15 ppm。
Lycopene, a kind of liposolubility carotenoids, has the strong hydrophobicity. The poor solubility of lycopene in water and water-containing food system seriously limits its utilization in food processing. Therefore, developing a water-dispersible lycopene product is of great importance . In this paper, the preparation of lycopene-containing microemulsion and the change of lycopene structure during microemulsification was studied, then the stability of the microemulsion and its application were investigated. The main contents are described as follow:
This paper studied the ingredients used to prepare the microemulsion, including oil to solubilize lycopene, kinds of emulsifier, co-emulsifier, Km and preparation temperature,which were investigated by single-factor experiments. The optimal formula and processing technology were screened via orthogonal experiments using microemulsion stability as an index. The result is that the optimal microemulsion system was composed of median chain triglyceride oil, Tween-40 and ethanol, the ratio of these ingredients was 1:5:8 (W:W:W). The concentration of lycopene in the new product is 4 mg/mL. The results of Particle size test indicate that the particle size of lycopene is 14.34 nm in average.
Based on the existing identification method of lycopene isomers,the change of lycopene structure was analyzed before and after microemulsion. By using the UV-Vis whole wavelength scanning and HPLC testing, isomers were detected after microemulsion. LC-MS analysis showed that main isomers were 9-Z and 13-Z. Before microemulsion, It proved that Z-lycopene and all-E were 7.33% and 92.67% respectively; after microemulsion, the system contained 55.5% Z-lycopene, which was improved significantly, and 44.5% all-E lycopene .
It was found that the addition of antioxidant in the process could reduce the degradation of lycopene. Based on the antioxidant activities and investigation of different antioxidants, the optimal antioxidant was determined as 0.1 g/kg L-ascorbic usions palmitate.
Storing lycopene emulsions in different conditions, including different temperature, avoid light/ light, air/flooding oxygen was also investigated. It was found that when the microemulsion were restored in 4℃, 25℃and 37℃for 60 days,the corresponding survival rate were 70.38%, 62.66% and 46.16%, respectively; the lycopene survival rates were 62.66%, 49.81% in avoid light and sun conditions stored 60 days, respectively; the lycopene survival rate were 48.76%, 82.26% when the lycopene was stored 60 days in the air, flooding oxygen conditions, respectively; In avoid light, flooding oxygen conditions, lycopene emulsion were respectively stayed in environments of 4℃and 25℃, after 30 days, there still remaining above 90% in 4℃. After 60 days, the survival rate was 84.9%. In the 25℃stored 60 days, the survival rate is 79.86%, so that the best storage condition was: 4℃, avoid light, and with the protection of flooding oxygen. The deposit height ratio w was used as the evaluation index of the product quality and structure stability. After 10, 20 and 60 days, w was 0, 3.3% and 6%, respectively. It was proved that microemulsion could be stable and homogeneous in a certain period.
The lycopene-containing microemulsion could be used in drink which has the function of health care.
通过考察番茄红素在不同种类食用油、乳化剂、助乳化剂中的溶解情况,筛选出油相、乳化剂、助乳化剂的种类并确定Km值和配制温度范围;以乳化体系的稳定性为评价指标,采用正交实验对微乳的配方进行优化,确定番茄红素微乳体系的最优组合如下:选用中链甘油三酸酯为番茄红素的携带油脂,选用吐温40为乳化剂,选用乙醇为助乳化剂,确定番茄红素与中链甘油三酸酯的比例为1:3,表面活性剂和助表面活性剂的比例为吐温40:乙醇=11:6;确定微乳中油相、乳化剂混合物、水的质量比为1:5:8。该工艺下制备出含番茄红素微乳中番茄红素的含量可达4 mg/mL,粒径检测结果表明,微乳中番茄红素颗粒的Z-Ave粒径为14.34 nm。
依据现有的番茄红素异构体鉴定方法,分析微乳形成前后体系内番茄红素的结构变化。通过紫外-可见分光光度计全波长扫描,HPLC检测均显示微乳中有异构体产生; LC-MS分析证实在微乳化过程中产生的异构体主要是9-Z和13-Z。构型组成分析结果表明,处理前番茄红素以全反式为主,顺式构型和全反式构型所占比例分别是7.33%和92.67%;经过微乳化处理后,番茄红素中顺式构型所占比例为55.5%,全反式构型所占比例为44.5%。
通过分析发现,添加抗氧化剂可降低水分散型番茄红素微乳中番茄红素降解速率。通过考察不同种抗氧化剂抗氧化性以及对水分散型番茄红素微乳的影响,确定抗氧化剂的种类及用量为0.1 g/kg的L-抗坏血酰棕榈酸酯。
通过对水分散型番茄红素微乳在不同温度,避光/日光,有氧/驱氧条件下存放过程中番茄红素保留率变化的研究发现,在4℃、25℃、37℃下贮藏60天后,微乳中番茄红素的含量分别为:70.38%、62.66%、46.16%;在避光和日光条件下贮藏60天,微乳中番茄红素的含量分别为:62.66%、49.81%;在有氧、驱氧条件下贮藏60天,微乳中番茄红素的含量分别为:48.76%、82.26%;在避光条件下,将驱氧的水分散型番茄红素微乳分别贮藏于4℃和25℃环境中,4℃贮藏30天时保留率仍维持在90%以上,贮藏60天时,保留率为84.9%。在25℃贮藏60天,保留率为79.86%,由此得出最佳贮藏条件为:将水分散型番茄红素微乳在4℃避光驱氧保存。通过离心实验观察产品的质构稳定性,以沉积高度比w值为评价指标,可知当水分散型番茄红素微乳贮藏至10天、20天、60天时,w值分别为:0、3.3%、6%,证明微乳在一定时间内质构均一稳定。
将所制备的水分散型番茄红素微乳应用到饮料方面,配制出一种具有保健功能的新型饮料,其中番茄红素含量为15 ppm。
Lycopene, a kind of liposolubility carotenoids, has the strong hydrophobicity. The poor solubility of lycopene in water and water-containing food system seriously limits its utilization in food processing. Therefore, developing a water-dispersible lycopene product is of great importance . In this paper, the preparation of lycopene-containing microemulsion and the change of lycopene structure during microemulsification was studied, then the stability of the microemulsion and its application were investigated. The main contents are described as follow:
This paper studied the ingredients used to prepare the microemulsion, including oil to solubilize lycopene, kinds of emulsifier, co-emulsifier, Km and preparation temperature,which were investigated by single-factor experiments. The optimal formula and processing technology were screened via orthogonal experiments using microemulsion stability as an index. The result is that the optimal microemulsion system was composed of median chain triglyceride oil, Tween-40 and ethanol, the ratio of these ingredients was 1:5:8 (W:W:W). The concentration of lycopene in the new product is 4 mg/mL. The results of Particle size test indicate that the particle size of lycopene is 14.34 nm in average.
Based on the existing identification method of lycopene isomers,the change of lycopene structure was analyzed before and after microemulsion. By using the UV-Vis whole wavelength scanning and HPLC testing, isomers were detected after microemulsion. LC-MS analysis showed that main isomers were 9-Z and 13-Z. Before microemulsion, It proved that Z-lycopene and all-E were 7.33% and 92.67% respectively; after microemulsion, the system contained 55.5% Z-lycopene, which was improved significantly, and 44.5% all-E lycopene .
It was found that the addition of antioxidant in the process could reduce the degradation of lycopene. Based on the antioxidant activities and investigation of different antioxidants, the optimal antioxidant was determined as 0.1 g/kg L-ascorbic usions palmitate.
Storing lycopene emulsions in different conditions, including different temperature, avoid light/ light, air/flooding oxygen was also investigated. It was found that when the microemulsion were restored in 4℃, 25℃and 37℃for 60 days,the corresponding survival rate were 70.38%, 62.66% and 46.16%, respectively; the lycopene survival rates were 62.66%, 49.81% in avoid light and sun conditions stored 60 days, respectively; the lycopene survival rate were 48.76%, 82.26% when the lycopene was stored 60 days in the air, flooding oxygen conditions, respectively; In avoid light, flooding oxygen conditions, lycopene emulsion were respectively stayed in environments of 4℃and 25℃, after 30 days, there still remaining above 90% in 4℃. After 60 days, the survival rate was 84.9%. In the 25℃stored 60 days, the survival rate is 79.86%, so that the best storage condition was: 4℃, avoid light, and with the protection of flooding oxygen. The deposit height ratio w was used as the evaluation index of the product quality and structure stability. After 10, 20 and 60 days, w was 0, 3.3% and 6%, respectively. It was proved that microemulsion could be stable and homogeneous in a certain period.
The lycopene-containing microemulsion could be used in drink which has the function of health care.
引文
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2.惠伯棣.类胡萝卜素化学及生物化学[M].中国轻工业出版社, 2005: 1-5
3.李福枝,刘飞,曾晓希,等.天然类胡萝卜素的研究进展[J].食品工业科技, 2007, 28(9): 227-232
4.张连富.番茄红素开发及生理功能研究[D]: [博士论文].无锡:无锡轻工业大学, 2000
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