超声耦合双水相体系提取茶皂素的工艺优化与机制探讨

doi:10.3864/j.issn.0578-1752.2022.01.014

中国农业科学 ›› 2022, Vol. 55 ›› Issue (1): 167-183.doi: 10.3864/j.issn.0578-1752.2022.01.014

超声耦合双水相体系提取茶皂素的工艺优化与机制探讨

杜金婷^1,²(),张雁¹(),李雁²,王佳佳¹,廖娜¹,钟立煌¹,骆碧群³,林江³

¹广东省农业科学院蚕业与农产品加工研究所/农业农村部功能食品重点实验室/广东省农产品加工重点实验室,广州 510610
²华南农业大学食品学院,广州 510640
³广东星汇生物科技有限公司,广东龙川 517323

收稿日期:2021-05-26 接受日期:2021-09-13 出版日期:2022-01-01 发布日期:2022-01-07
通讯作者: 张雁
作者简介:杜金婷,E-mail： 3046023329@qq.com。
基金资助:
广东省本土创新创业团队项目(2019BT02N112);广东省现代农业产业技术体系创新团队建设专项资金(2020KJ117);广东省农业科学院农业优势产业学科团队建设项目(202108TD)

Optimization and Mechanism of Ultrasonic-Assisted Two-Phase Extraction of Tea Saponin

DU JinTing^1,²(),ZHANG Yan¹(),LI Yan²,WANG JiaJia¹,LIAO Na¹,ZHONG LiHuang¹,LUO BiQun³,LIN Jiang³

¹Sericultural & Agri-Food Research Institute, Guangdong Academy of Agricultural Sciences/Key Laboratory of Functional Foods, Ministry of Agriculture and Rural Affairs/Guangdong Key Laboratory of Agricultural Products Processing, Guangzhou 510610
²College of Food Science, South China Agricultural University, Guangzhou 510640
³Guangdong Xinghui Biological Technology Co., Ltd., Longchuan 517323, Guangdong

Received:2021-05-26 Accepted:2021-09-13 Online:2022-01-01 Published:2022-01-07
Contact: Yan ZHANG

摘要/Abstract

摘要：

【目的】茶皂素是一种具有广阔应用前景的天然活性物质,纯度是限制其应用和价值的关键因素。探究超声耦合双水相提取（Ultrasound-assisted two-phase aqueous extraction, UAATPE）油茶粕茶皂素的工艺条件及其提取机制,以开发纯度高且高效的提取技术,为油茶粕高值化利用提供技术指导。【方法】以油茶粕为原料,在单因素基础上,利用Plackett-Burman设计筛选影响得率的关键因素,经Box-Behnken设计优化提取工艺;通过比较传统乙醇提取法和水提法的提取物得率和纯度,评价UAATPE法茶皂素提取效果;结合扫描电子显微镜分析油茶粕微观结构,初步探讨UAATPE法提取机制。【结果】影响茶皂素得率的关键因素为乙醇质量分数、硫酸铵质量分数和超声时间,经Box-Behnken设计优化的最佳工艺参数为：乙醇质量分数27.50%（w/w）,硫酸铵质量分数19.60%（w/w）,液固比50﹕1,超声时间32 min,超声功率300 W,提取温度60℃,在此条件下茶皂素得率为（26.21±0.54）%。与传统乙醇提取法相比,UAATPE法的茶皂素得率虽差异不显著,但其纯度提高了6.57%（P<0.05）。相较于传统水提法,UAATPE法提取的茶皂素得率和纯度分别提升了17.74%和40.23%（P<0.01）。微观结构显示UAATPE法处理的油茶粕因超声波空化效应,加剧了油茶粕组织破坏,产生大量空洞和强烈表面收缩,有效促进油茶粕茶皂素释放。UAATPE提取过程,茶皂素在双水相系统中首先经过固液提取进入电导率高的底相,然后经液液萃取迁移至极性较大的顶相,从而达到初级纯化,提升茶皂素纯度的效果。【结论】采用UAATPE法可以显著提高茶皂素得率和纯度,为油茶粕的高效利用提供了新方法。

关键词: 油茶粕, 茶皂素, 超声波, 双水相提取, Plackett-Burman设计, 响应面设计

Abstract:

【Objective】 Tea saponin is a naturally active substance with wide application prospective, and its purity is the key factor limiting its application and value. In this study, the optimal conditions for ultrasonic-assisted two-phase extraction (UAATPE) of tea saponin from camellia meal were explored, and the possible extraction mechanism was discussed in order to develop an efficient, high-purity extraction technology, so as to provide a technical guidance for high-value utilization of camellia meal. 【Method】 On the basis of the single factor experimental results, the key factors affecting the yield of tea saponin were screened by Plackett Burman design, and the extraction process was optimized by Box-Behnken design. The extraction efficiency of tea saponin using the UAATPE method was evaluated by comparing the extraction yield and purity to the traditional ethanol extraction method and water extraction method. Scanning electron microscopy (SEM) was employed to analyze the microstructure of camellia meal, and the possible mechanism of extraction by the UAATPE method was discussed. 【Result】 The key factors affecting the yield of tea saponin were mass fraction of ethanol, mass fraction of ammonium sulfate, and ultrasonic time. The process parameters optimized by Box-Behnken design were as follows: an ethanol content of 27.50% (W/W), an ammonium sulfate content of 19.60% (W/W), a liquid-solid ratio of 50﹕1, an ultrasonic time of 32 min, an ultrasonic power of 300 W and an extraction temperature of 60℃, and the yield of tea saponin at (26.21±0.54)% was achieved under the optimized conditions. Compared with the traditional method of ethanol extraction, the purity of tea saponin extracted by the UAATPE method increased by 6.57% (P<0.05), although the difference of the yield of tea saponin extracted by these two methods was not significant. Compared with the traditional method of water extraction, the yield and purity of tea saponin extracted using the UAATPE method were increased by 17.74% and 40.23%, respectively (P<0.01). The microstructure showed that owing to the effect of the camellia meal treated by the UAATPE method, the ultrasonic cavitation accelerated the tissue damage of the camellia meal, producing a large number of voids and strong surface shrinkage, which effectively promoted the release of tea saponin in the camellia meal. In the process of the UAATPE extraction, the tea saponin first entered the bottom phase with high electrical conductivity through solid-liquid extraction in the two-phase water system, and then moved to the top phase with high polarity through liquid-liquid extraction, achieving primary purification and improving the purity of tea saponin. 【Conclusion】 The UAATPE method could significantly improve the yield and purity of tea saponin, thus providing a new novel method for the efficient utilization of camellia meal.

Key words: camellia meal, tea saponin, ultrasound, aqueous two-phase extraction, Plackett-Burman, response surface design

杜金婷,张雁,李雁,王佳佳,廖娜,钟立煌,骆碧群,林江. 超声耦合双水相体系提取茶皂素的工艺优化与机制探讨[J]. 中国农业科学, 2022, 55(1): 167-183.

DU JinTing,ZHANG Yan,LI Yan,WANG JiaJia,LIAO Na,ZHONG LiHuang,LUO BiQun,LIN Jiang. Optimization and Mechanism of Ultrasonic-Assisted Two-Phase Extraction of Tea Saponin[J]. Scientia Agricultura Sinica, 2022, 55(1): 167-183.

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水平Level	A 乙醇质量分数 Concentration of ethanol (%)	B 硫酸铵质量分数 Concentration of ammonium sulphate (%)	C 液固比 Solvent-to-material ratio	D 提取温度 Extraction temperature (℃)	E 功率 Ultrasonic power (W)	F 超声时间 Ultrasonic time (min)
-1	26	18	40﹕1	50	250	20
+1	30	22	60﹕1	70	350	40

试验顺序 Test no.	A	B	C	D	E	F	茶皂素得率 Tea saponin yield (%)
1	+1	-1	+1	+1	+1	-1	22.58
2	-1	-1	-1	-1	-1	-1	22.88
3	+1	+1	-1	+1	+1	+1	18.97
4	-1	+1	+1	+1	-1	-1	22.10
5	+1	+1	+1	-1	-1	-1	19.74
6	-1	+1	+1	-1	+1	+1	19.51
7	-1	-1	+1	-1	+1	+1	22.76
8	-1	+1	-1	+1	+1	-1	22.54
9	+1	-1	-1	-1	+1	-1	21.34
10	-1	-1	-1	+1	-1	+1	21.26
11	+1	+1	-1	-1	-1	+1	18.57
12	+1	-1	+1	+1	-1	+1	19.98

方差来源 Sources of variation	平方和 Quadratic sum	自由度 DOF	均方 Mean square	F值 F value	P值 P value
模型 Model	25.50	6	4.25	9.40	0.0132
乙醇质量分数 Concentration of ethanol	8.12	1	8.12	17.96	0.0082
硫酸铵质量分数 Concentration of ammonium sulphate	7.32	1	7.32	16.18	0.0101
液固比 Solvent-to-material ratio	0.10	1	0.10	0.23	0.6538
提取温度 Temperature	0.58	1	0.58	1.28	0.3101
功率 Ultrasonic power	0.84	1	0.84	1.85	0.2316
超声时间 Ultrasonic time	8.55	1	8.55	18.92	0.0074
残差 Residual	2.26	5	0.45
总差 Total	27.76	11
R²	0.9186	R²_Adj	0.8209	R²_Pred	0.5310

参数 Parameter	平方和 Quadratic sum	自由度 DOF	均方 Mean square	F值 F value	P值 P value	显著性 Significance
模型Model	44.46	9	4.94	61.17	<0.0001	**
x₁	1.71	1	1.71	21.19	0.0025	**
x₂	1.14	1	1.14	14.12	0.0071	**
x₃	0.52	1	0.52	6.44	0.0388	*
x₁x₂	7.65	1	7.65	94.68	<0.0001	**
x₁x₃	1.05	1	1.05	13.01	0.0087	**
x₂x₃	0.055	1	0.055	0.68	0.4355
x₁²	11.07	1	11.07	137.05	<0.0001	**
x₂²	15.70	1	15.70	194.48	<0.0001	**
x₃²	2.60	1	2.60	32.23	0.0008	**
残差 Residual	0.57	7	0.081
失拟项 Lack of fit	0.14	3	0.045	0.42	0.7464
纯误差 Pure error	0.43	4	0.11
总和 Total	45.02	16

方法 Method	溶剂 Solvent	提取条件 Extraction condition			得率 Yield (%)	纯度 Purity (%)
方法 Method	溶剂 Solvent	时间 Time (min)	温度 Temperature (℃)	液固比 Solvent-to-material	得率 Yield (%)	纯度 Purity (%)
乙醇提取法 Ethanol extraction	80%乙醇 80% ethanol	60	80	10:1	27.02±0.37a	62.01±0.03b
水提法 Water extraction	H₂O	60	80	10:1	22.26±0.99b	47.13±0.06c
超声波辅助双水相提取法 UAATPE	27.50%乙醇/19.60%硫酸铵 27.50% ethanol/19.60% ammonium sulphate	32	60	50:1	26.21±0.54a	66.09±0.04a

超声耦合双水相体系提取茶皂素的工艺优化与机制探讨

Optimization and Mechanism of Ultrasonic-Assisted Two-Phase Extraction of Tea Saponin

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流动相 Mobile phase	时间 Time (min)
流动相 Mobile phase	0	25	35	40	45
A：甲醇 A: Methanol	10	60	62	70	72
B：0.4%乙酸溶液 B: 0.4% acetic acid solution	90	40	38	30	28

因素 Factor	水平 Level
因素 Factor	-1	0	+1
乙醇质量分数 Concentration of ethanol (x₁, %)	26	28	30
硫酸铵质量分数 Concentration of ammonium sulphate (x₂, %)	18	20	22
超声时间 Ultrasonic time (x₃, min)	20	30	40

标准顺序 Standard	试验顺序 Test no.	乙醇质量分数 Concentration of ethanol x₁	盐质量分数 Concentration of ammonium sulphate x₂	超声时间 Ultrasonic time x₃	茶皂素得率 Tea saponin yield (%)
11	1	30	20	20	24.04
15	2	28	22	20	23.20
13	3	28	20	30	26.85
14	4	28	20	30	26.35
5	5	28	20	30	26.75
6	6	28	20	30	26.12
10	7	28	20	30	26.83
3	8	28	22	40	24.01
9	9	26	18	30	25.41
2	10	30	18	30	21.64
12	11	28	18	20	23.95
7	12	26	20	20	23.86
8	13	26	20	40	25.33
17	14	30	22	30	23.41
4	15	26	22	30	21.65
16	16	30	20	40	23.46
1	17	28	18	40	24.29

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