响应面法优化辣椒籽油碱异构化制备共轭亚油酸工艺及其氧化稳定性

doi:10.6048/j.issn.1001-4330.2022.04.015

新疆农业科学 ›› 2022, Vol. 59 ›› Issue (4): 908-915.DOI: 10.6048/j.issn.1001-4330.2022.04.015

• 园艺特产·农产品加工工程 • 上一篇下一篇

响应面法优化辣椒籽油碱异构化制备共轭亚油酸工艺及其氧化稳定性

马燕¹(), 许铭强¹, 李喜弟², 孟新涛¹, 邹淑萍¹, 张婷¹, 张谦¹()

1.新疆农科院农产品贮藏加工研究所/新疆主要农副产品精深加工工程技术研究中心,乌鲁木齐 830091
2.新疆西尔单食品有限公司,乌鲁木齐 830091

收稿日期:2021-10-05 出版日期:2022-04-20 发布日期:2022-04-24
通信作者: 张谦
作者简介:马燕(1984-),山东济南人,女,副研究员,博士,研究方向为农产品精深加工及副产物综合利用,(E-mail) mayan101314@sina.com
基金资助:
农业部公益性行业科研专项“蔬菜副产物综合利用技术研究与示范”(201303079);农业部果蔬加工重点实验室开放基金项目“不同处理改性辣椒籽膳食纤维的特性研究”(GSKF2016003);新疆维吾尔自治区自然科学青年基金项目“超高压对辣椒籽蛋白特性的影响及其机理研究”(2016D01B031)

Optimization of Preparation of Conjugated Linoleic Acid by Alkali Isomerization of Pepper Seed Oil by Response Surface Methodology and Its Oxidation Stability

MA Yan¹(), XU Mingqiang¹, LI Xidi², MENG Xintao¹, ZOU Shuping¹, ZHANG Ting¹, ZHANG Qian¹()

1. Institute of Farm Product Storage and Processing, Xinjiang Academy of Agricultural Sciences /Research Center of Xinjiang Main Farm Products Processing Engineering, Urumqi 830091,China
2. Xinjiang Xierdan Food Co., Ltd., Urumqi 830091,China

Received:2021-10-05 Online:2022-04-20 Published:2022-04-24
Correspondence author: ZHANG Qian
Supported by:
Special Fund for Public Welfare Industry (Agriculture) Scientific R & D Program of Ministry of Agriculture "Research and Demonstration of Comprehensive Utilization Technology of Vegetable By-Products"(201303079);Open Fund Project of Key Laboratory of Fruit and Vegetable Processing of Ministry of Agriculture "Study on the Characteristics of Modified Pepper Seed Dietary Fiber"(GSKF2016003);Xinjiang Natural Fund Project "Effect of High Pressure on the Properties of Pepper Seed Protein and Its Mechanism "(2016D01B031)

摘要/Abstract

摘要：

【目的】研究碱异构化法制备辣椒籽油共轭亚油酸工艺,得到高转化率的辣椒籽油共轭亚油酸,为辣椒副产物综合利用及制备共轭亚油酸的新资源开发提供理论依据。【方法】以共轭亚油酸转化率为指标,以反应时间、反应温度、碱油比和溶油比为主要影响因素,运用响应面中心组合设计(CCD),分析不同因素对辣椒籽油共轭亚油酸转化率的影响,研究辣椒籽油共轭亚油酸的制备工艺,采用Schaal加速试验对比辣椒籽油与辣椒籽油共轭亚油酸的氧化稳定性。【结果】辣椒籽油共轭亚油酸最佳工艺参数:反应温度为169℃,反应时间为 4.4 h,碱油比[M_(KOH)∶M_{(辣椒籽油)}]为0.2,溶油比[M_{(聚乙二醇)}∶M_{(辣椒籽油)} ]为1.7时,共轭转化率可达84.60%,其氧化稳定性优于辣椒籽油。【结论】响应面优化法优化碱异构化制备辣椒籽油共轭亚油酸工艺可得到较高转化率、稳定性较好的辣椒籽油共轭亚油酸。

关键词: 辣椒籽油; 碱异构化; 响应面优化; 共轭亚油酸; 氧化稳定性

Abstract:

【Objective】 To study the preparation of conjugated linoleic acid from pepper seed oil by isomerization alkali in order to obtain high conversion of pepper seed oil conjugated linoleic acid.【Method】 The Conversion Rate of Conjugated Linoleic Acid was used as an indicator of investigation, the main influencing factors were reaction time, reaction temperature, alkali oil ratio and dissolved oil ratio, and the effects of different factors on conjugated linoleic acid conversion of pepper seed oil was analyzed by CCD. After that, the preparation process of conjugated linoleic acid from capsicum seed oil was determined, and the oxidation stability of conjugated linoleic acid between pepper seed oil and pepper seed oil was compared by Schaal oven accelerated test.【Result】 The optimal technical conditions are determined as follows by establishing the quadratic response regression model: The reaction temperature was 169℃, the reaction time was 4.4 h, Alkali oil ratio [M(KOH):M (Pepper seed oil)] was 0.2, Dissolved oil ratio [M(polyethylene glycol):M(Pepper seed oil)] was 1.7, and the conjugation conversion could reach 84.60%. Its oxidation stability was better than that of pepper seed oil.【Conclusion】 The process conditions of conjugated linoleic acid in pepper seed oil are optimized by response surface methodology, and the conjugated linoleic acid in pepper seed oil with good stability is obtained.

Key words: pepper seed oil; response surface optimization; alkali isomerization; conjugated linoleic acid; oxidation stability

马燕, 许铭强, 李喜弟, 孟新涛, 邹淑萍, 张婷, 张谦. 响应面法优化辣椒籽油碱异构化制备共轭亚油酸工艺及其氧化稳定性[J]. 新疆农业科学, 2022, 59(4): 908-915.

MA Yan, XU Mingqiang, LI Xidi, MENG Xintao, ZOU Shuping, ZHANG Ting, ZHANG Qian. Optimization of Preparation of Conjugated Linoleic Acid by Alkali Isomerization of Pepper Seed Oil by Response Surface Methodology and Its Oxidation Stability[J]. Xinjiang Agricultural Sciences, 2022, 59(4): 908-915.

图/表 7

图1 自制共轭亚油酸反应装置

Fig.1 Reaction diagram of conjugated linoleic acid by self-made device

表1 因素与水平

Table 1 Factors and levels of response surface

自变量 Independent variable	编码值 Coded value	编码水平 Coding level
自变量 Independent variable	编码值 Coded value	-1	0	1
反应温度 Reaction temperature(℃)	X₁	160	170	180
反应时间 Reaction time(h)	X₂	3	4	5
碱油比 Alkali oil ratio	X₃	0.5	0.3	0.1
溶油比 Solvent oil ratio	X₄	1	1.5	2

表2 优化试验设计与结果

Table 2 Optimize experimental designs and results

处理号 Run seque-nce	反应温度 Reaction temperature(℃)	反应时间 Eaction time(h)	碱油比 Alkali oil ratio	溶油比 Solvent oil ratio	共轭转化率Y₁ Conjugate conversiont rate Y₁(%)
1	0	0	-1	1	84.62
2	0	1	0	1	74.56
3	-1	1	0	0	90.32
4	1	0	1	0	76.34
5	0	-1	1	0	85.42
6	-1	0	1	0	87.43
7	-1	0	-1	0	82.46
8	0	0	0	0	81.4
9	0	-1	-1	0	69.4
10	-1	-1	0	0	65.23
11	-1	0	0	1	78.6
12	1	-1	0	0	82.32
13	0	0	0	0	88.2
14	1	0	0	-1	80.12
15	0	0	1	-1	82.45
16	1	0	0	1	85.32
17	1	0	-1	0	81.5
18	0	-1	0	1	76.51
19	1	1	0	0	87.78
20	0	0	-1	-1	60.08
21	-1	0	0	-1	76.32
22	0	0	0	0	86.65
处理号 Run seque-nce	反应温度 Reaction temperature(℃)	反应时间 Eaction time(h)	碱油比 Alkali oil ratio	溶油比 Solvent oil ratio	共轭转化率Y₁ Conjugate conversiont rate Y₁(%)
23	0	0	1	1	78.96
24	0	1	0	-1	81.34
25	0	1	1	0	79.6
26	0	-1	0	-1	60.4
27	0	0	0	0	87.46
28	0	1	-1	0	83.52
29	0	0	0	0	86.44

表3 回归模型系数及显著性检验结果

Table 3 Regression coefficients and significant test for quadratic polynomial model equation

变异来源 Source	自由度 df	平方和 Sum of Squares	均方 Mean Square	F值 F-value	P P-value
模型Model	14	1 450.24	103.590	5.20	0.002 0^***
X₁	1	14.13	14.13	0.709 3	0.413 8
X₂	1	278.79	278.79	14.00	0.002 $2 * *$
X₃	1	68.26	68.26	3.43	0.085 3
X₄	1	119.45	119.45	6.00	0.028 1^*
X₁X₂	1	96.33	96.33	4.84	0.045 2^*
X₁X₃	1	25.65	25.65	1.29	0.275 5
X₁X₄	1	2.13	2.13	0.107 0	0.748 4
X₂X₃	1	99.40	99.40	4.99	0.042 3^*
X₂X₄	1	130.99	130.99	6.58	0.022 5^*
X₃X₄	1	196.42	101.40	9.86	0.007 $2 * *$
X₁₂	1	0.034 1	0.034 1	0.001 7	0.967 6
X₂₂	1	145.74	145.74	7.32	0.017 1^*
X₃₂	1	51.49	51.49	2.59	0.130 2
X₄₂	1	307.03	307.03	15.42	0.001 5^***
残差误差Residual	14	278.83	19.92	3.48	0.120 4
失拟Lack of Fit	10	250.09	25.01
纯误差总和 Cor Total	4 28	28.74 1 729.07	7.19
相关系数R²	0.838 7
变异系数CV	0.58

表3 回归模型系数及显著性检验结果

Table 3 Regression coefficients and significant test for quadratic polynomial model equation

变异来源 Source	自由度 df	平方和 Sum of Squares	均方 Mean Square	F值 F-value	P P-value
模型Model	14	1 450.24	103.590	5.20	0.002 0^***
X₁	1	14.13	14.13	0.709 3	0.413 8
X₂	1	278.79	278.79	14.00	0.002 $2 * *$
X₃	1	68.26	68.26	3.43	0.085 3
X₄	1	119.45	119.45	6.00	0.028 1^*
X₁X₂	1	96.33	96.33	4.84	0.045 2^*
X₁X₃	1	25.65	25.65	1.29	0.275 5
X₁X₄	1	2.13	2.13	0.107 0	0.748 4
X₂X₃	1	99.40	99.40	4.99	0.042 3^*
X₂X₄	1	130.99	130.99	6.58	0.022 5^*
X₃X₄	1	196.42	101.40	9.86	0.007 $2 * *$
X₁₂	1	0.034 1	0.034 1	0.001 7	0.967 6
X₂₂	1	145.74	145.74	7.32	0.017 1^*
X₃₂	1	51.49	51.49	2.59	0.130 2
X₄₂	1	307.03	307.03	15.42	0.001 5^***
残差误差Residual	14	278.83	19.92	3.48	0.120 4
失拟Lack of Fit	10	250.09	25.01
纯误差总和 Cor Total	4 28	28.74 1 729.07	7.19
相关系数R²	0.838 7
变异系数CV	0.58

图2 因子交互与共轭转化率的响应面图

Fig.2 Response surface diagram of factor interaction and conjugate conversion

图3 辣椒籽油和辣椒籽油CLA中过氧化值比较

Fig.3 Comparison of peroxide value between pepper seed oil and pepper seed oil CLA

图4 辣椒籽油和辣椒籽油CLA中TBA反应物比较

Fig.4 Comparison of TBA reactant between pepper seed oil and pepper seed oil CLA

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响应面法优化辣椒籽油碱异构化制备共轭亚油酸工艺及其氧化稳定性

Optimization of Preparation of Conjugated Linoleic Acid by Alkali Isomerization of Pepper Seed Oil by Response Surface Methodology and Its Oxidation Stability

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