Optimization of extraction process for soluble and insoluble dietary fibers from Ougan (Citrus suavissima Hort. ex Tanaka) pomace and the differences between their physicochemical properties and functional characteristics

doi:10.3969/j.issn.1004-1524.20240125

Acta Agriculturae Zhejiangensis ›› 2025, Vol. 37 ›› Issue (1): 189-202.DOI: 10.3969/j.issn.1004-1524.20240125

• Food Science • Previous Articles Next Articles

Optimization of extraction process for soluble and insoluble dietary fibers from Ougan (Citrus suavissima Hort. ex Tanaka) pomace and the differences between their physicochemical properties and functional characteristics

LIU Xun¹^,²(), XIA Qile², LI Yanpo³, WANG Yangguang¹^,^*(), LU Shengmin¹^,²^,^*()

1. School of Food and Pharmacy, Zhejiang Ocean University, Zhoushan 316022, Zhejiang, China
2. Provincial Key Laboratory of Fruit and Vegetable Preservation and Processing Technology, Key Laboratory of Postharvest Fruit Processing of the Ministry of Agriculture and Rural Affairs, Institute of Food Science, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
3. Institute of Food Science, Wenzhou Academy of Agricultural Sciences, Wenzhou 325000, Zhejiang, China

Received:2024-02-04 Online:2025-01-25 Published:2025-02-14

Abstract

Abstract:

To further improve the comprehensive utilization rate and functional value of Ougan pomace resources, freshly squeezed citrus pomace was used as raw material, and ultrasound assisted cellulase method was adopted to extract its soluble dietary fiber (SDF) and insoluble dietary fiber (IDF). Single factor experiments and response surface methodology were used to optimize the process parameters and their in vitro physicochemical properties and functional characteristics were explored and compared. The results showed that under the process conditions of solid-liquid ratio of 1∶20 (g·mL^-1), ultrasound power of 450 W, cellulase addition of 0.97%, and enzymatic hydrolysis time of 1 h, the extraction rates of SDF and IDF were (10.42±0.31)% and (51.28±0.97)%, respectively. SDF appeared multiple folds on surface while IDF’ appearance looked smoother and had more pores and holes, which caused significant difference in their physicochemical properties and functional characteristics. Compared to IDF, SDF had higher water-holding and swelling capacities but lower oil-holding capacity (P<0.05). Significantly (P<0.05) higher glucose adsorbing capacity and α-glucosidase inhibiting capacity were found in SDF than those in IDF, and both had the best delay effect on glucose dialysis within 30 min, with highest peak glucose dialysis retardation index (GDRI) (32.73±0.89)% existed in SDF. Both SDF and IDF effectively adsorbed cholesterol and cholate in the simulated small intestinal environment, and SDF showed better adsorption ability to cholesterol and glycocholate than IDF. SDF had a significantly (P <0.05) higher adsorption capacity for nitrite ions than IDF in the simulated gastric environment. In conclusion, the results indicated that dietary fibers in Ougan pomace had strong functional activity in vitro, especially significantly excellent performance found for SDF to adsorb glucose, lipid and nitrite, and could be used for subsequent in vivo function verification and functional food development.

Key words: Ougan pomace, soluble dietary fiber, insoluble dietary fiber, ultrasound assisted enzymatic extraction, physicochemical property, functional characteristic

CLC Number:

TS209

LIU Xun, XIA Qile, LI Yanpo, WANG Yangguang, LU Shengmin. Optimization of extraction process for soluble and insoluble dietary fibers from Ougan (Citrus suavissima Hort. ex Tanaka) pomace and the differences between their physicochemical properties and functional characteristics[J]. Acta Agriculturae Zhejiangensis, 2025, 37(1): 189-202.

Figures/Tables 11

Table 1 Design parameters of the response surface experiment

水平 Level	因素Factor
水平 Level	A纤维素酶添加量 Enzyme addition amount/%	B酶解时间 Enzymatic hydrolysis time/h	C超声功率 Ultrasonic power/W
-1	0.6	0.5	400
0	0.8	1	450
1	1.0	1.5	500

Fig.1 Analysis of single factor test results SDF,Soluble dietary fiber.Different lowercase letters indicate significant differences (P<0.05) among different teatments. The same as below.

Table 2 Response surface test results

序号 Serial number	A酶添加量 Enzyme addition amount/%	B酶解时间 Enzymatic hydrolysis time/h	C超声功率 Ultrasonic power/W	SDF提取率 Extraction rate of SDF/%	IDF提取率 Extraction rate of IDF/%
1	0.6	0.5	450	7.32	50.47
2	1.0	0.5	450	8.32	50.50
3	0.6	1.5	450	8.80	49.63
4	0.6	1.0	450	8.95	49.78
5	0.6	1.0	400	7.12	48.61
6	1.0	1.0	400	7.21	49.59
7	0.6	1.0	500	7.62	48.90
8	1.0	1.0	500	7.97	50.55
9	0.8	0.5	400	6.51	50.17
10	0.8	1.5	400	7.17	48.13
11	0.8	0.5	500	7.53	50.26
12	0.8	1.5	500	8.21	49.78
13	0.8	1.0	450	9.90	51.13
14	0.8	1.0	450	10.45	49.91
15	0.8	1.0	450	11.20	51.24
16	0.8	1.0	450	10.10	51.31
17	0.8	1.0	450	9.99	52.66

Table 3 Analysis of variance of regression model

方差来源 Source of variance	平方和 Sum of squares	自由度 Degree of freedom	均方 Mean square	F值 F value	提取率Extraction rate
方差来源 Source of variance	平方和 Sum of squares	自由度 Degree of freedom	均方 Mean square	F值 F value	P值 P value	显著性 Significance
模型Modle	29.56	9	3.28	16.99	0.000 6	**
A酶添加量Enzyme addition amount	0.321 6	1	0.321 6	1.66	0.238 1
B酶解时间Enzymatic hydrolysis time	1.48	1	1.48	7.66	0.027 8	*
C超声功率Ultrasonic power	1.38	1	1.38	7.16	0.031 7	*
AB	0.180 5	1	0.180 5	0.934 0	0.366 0
AC	0.016 5	1	0.016 5	0.085 2	0.778 8
BC	0.000 1	1	0.000 1	0.000 4	0.984 4
A²	3.62	1	3.62	18.72	0.003 5	*
B²	4.69	1	4.69	24.24	0.001 7	*
C²	15.49	1	15.49	80.12	<0.000 1	**
残差Residual error	1.35	7	0.193 3
失拟项Lack of fit	0.219 9	3	0.073 3	0.258 7	0.852 2	不显著
						Not significant
净误差Net error	1.13	4	0.283 3
总离差Total dispersion	30.91	16
R²=0.956 2			$R_{A d j}^{2}$ =0.900 0	$R_{P r e}^{2}$ =0.828 9

Table 3 Analysis of variance of regression model

方差来源 Source of variance	平方和 Sum of squares	自由度 Degree of freedom	均方 Mean square	F值 F value	提取率Extraction rate
方差来源 Source of variance	平方和 Sum of squares	自由度 Degree of freedom	均方 Mean square	F值 F value	P值 P value	显著性 Significance
模型Modle	29.56	9	3.28	16.99	0.000 6	**
A酶添加量Enzyme addition amount	0.321 6	1	0.321 6	1.66	0.238 1
B酶解时间Enzymatic hydrolysis time	1.48	1	1.48	7.66	0.027 8	*
C超声功率Ultrasonic power	1.38	1	1.38	7.16	0.031 7	*
AB	0.180 5	1	0.180 5	0.934 0	0.366 0
AC	0.016 5	1	0.016 5	0.085 2	0.778 8
BC	0.000 1	1	0.000 1	0.000 4	0.984 4
A²	3.62	1	3.62	18.72	0.003 5	*
B²	4.69	1	4.69	24.24	0.001 7	*
C²	15.49	1	15.49	80.12	<0.000 1	**
残差Residual error	1.35	7	0.193 3
失拟项Lack of fit	0.219 9	3	0.073 3	0.258 7	0.852 2	不显著
						Not significant
净误差Net error	1.13	4	0.283 3
总离差Total dispersion	30.91	16
R²=0.956 2			$R_{A d j}^{2}$ =0.900 0	$R_{P r e}^{2}$ =0.828 9

Fig.2 Effect of each factor interaction on the extraction rate of soluble dietary fiber

Fig.3 SEM analysis of Ougan pomace, soluble dietary fiber and insoluble dietary fiber A, Ougan pomace at 600×; B, Ougan pomace at 2 000×; C, Soluble dietary fiber at 600×; D, Soluble dietary fiber at 2 000×; E, Insoluble dietary fiber at 600×; F, Insoluble dietary fiber at 2 000×.

Table 4 Analyses of physicochemical properties and functional characteristics of dietary fibers from Ougan pomace

材料 Material	持水力 Water holding capacity/ (g·g^-1)	膨胀力 Expandability/ (mL·g^-1)	持油力 Oil holding capacity/ (g·g^-1)
SDF	25.63±0.23 a	10.08±0.11 a	4.41±0.21 b
IDF	15.20±0.42 b	7.56±0.24 b	10.27±0.47 a
瓯柑果渣	12.74±0.26 c	1.67±0.05 c	3.94±0.28 b
Ougan pomace

Fig.4 Glucose dialysis retardation index of dietary fibers from Ougan pomace SDF, Soluble dietary fiber; IDF, Insoluble dietary fiber. The bars marked without the same lowercase letter indicated significant differences at P<0.05. The same as below.

Fig.5 α-Glucosidase inhibitory ability of dietary fibers from Ougan pomace

Fig.6 Cholesterol adsorption capacity and cholate adsorption rate of dietary fibers from Ougan pomace

Fig.7 Nitrite adsorption capacities of dietary fibers from Ougan pomace

References 31

[1]	张温翔. 温州市瓯海区瓯柑产业发展研究[D]. 南昌: 江西农业大学, 2023.
	ZHANG W X. Research on the development of Ou citrus industry in Ouhai District, Wenzhou City[D]. Nanchang: Jiangxi Agricultural University, 2023. (in Chinese with English abstract)
[2]	刘洵, 王阳光, 夏其乐, 等. 瓯柑功能性成分利用现状及深加工研究进展[J]. 食品与机械, 2022, 38(12): 226-231.
	LIU X, WANG Y G, XIA Q L, et al. Research progress on utilization status and deep processing of functional components of Ougan Citrus[J]. Food & Machinery, 2022, 38(12): 226-231. (in Chinese with English abstract)
[3]	杨学嘉. 晚清至民国温州瓯柑运销体制的转变[D]. 上海: 华东师范大学, 2019.
	YANG X J. Transformation of transportation and marketing system of Ougan (Citrus suavissima Hort. ex Tanaka) from late Qing dynasty to the Republic of China in Wenzhou[D]. Shanghai: East China Normal University, 2019. (in Chinese with English abstract)
[4]	联合国粮食及农业组织, 世界卫生组织. 营养标识准则: CXG2—1985[S]. 1985.
[5]	WEN J J, LI M Z, HU J L, et al. Different dietary fibers unequally remodel gut microbiota and charge up anti-obesity effects[J]. Food Hydrocolloids, 2023, 140: 108617.
[6]	GE Y F, WEI C H, RAJAVEL ARUMUGAM U, et al. Quinoa bran insoluble dietary fiber-zinc chelate mediates intestinal flora structure to regulate glucose and lipid metabolism in obese rats[J]. Journal of Functional Foods, 2023, 108: 105765.
[7]	SIDDIQUI H, SULTAN Z, YOUSUF O, et al. A review of the health benefits, functional properties, and ultrasound-assisted dietary fiber extraction[J]. Bioactive Carbohydrates and Dietary Fibre, 2023, 30: 100356.
[8]	BAI X L, HE Y, QUAN B Y, et al. Physicochemical properties, structure, and ameliorative effects of insoluble dietary fiber from tea on slow transit constipation[J]. Food Chemistry: X, 2022, 14: 100340.
[9]	XIE L, ALAM M J, MARQUES F Z, et al. A major mechanism for immunomodulation: dietary fibres and acid metabolites[J]. Seminars in Immunology, 2023, 66: 101737.
[10]	GARCIA-AMEZQUITA L E, TEJADA-ORTIGOZA V, SERNA-SALDIVAR S O, et al. Dietary fiber concentrates from fruit and vegetable by-products: processing, modification, and application as functional ingredients[J]. Food and Bioprocess Technology, 2018, 11(8): 1439-1463.
[11]	周永升, 莫小群, 张文婷, 等. 超声辅助纤维素酶法制备蔗叶膳食纤维及其理化特性分析[J]. 中国饲料, 2022(22): 107-113.
	ZHOU Y S, MO X Q, ZHANG W T, et al. Ultrasonic-assisted cellulase preparation of dietary fiber from sugarcane leaves and its physicochemical properties[J]. China Feed, 2022(22): 107-113. (in Chinese with English abstract)
[12]	黎素玲, 滕聪, 刘金阁, 等. 条斑紫菜可溶性膳食纤维的理化性质及体外生物活性研究[J]. 食品安全质量检测学报, 2023, 14(22): 9-18.
	LI S L, TENG C, LIU J G, et al. Study on the physicochemical properties and in vitro biological activities of soluble dietary fiber from Porphyra yezoensis[J]. Journal of Food Safety & Quality, 2023, 14(22): 9-18. (in Chinese with English abstract)
[13]	宫春宇, 廉雅雯, 于洋, 等. 玉米须不溶性膳食纤维分析及其对面包品质和消化特性的影响研究[J]. 中国调味品, 2024, 49(1): 67-73.
	GONG C Y, LIAN Y W, YU Y, et al. Analysis of corn silk insoluble dietary fiber and its effects on quality and digestion characteristics of bread[J]. China Condiment, 2024, 49(1): 67-73. (in Chinese with English abstract)
[14]	刘东杰, 周心雨, 王锋, 等. 麻竹笋壳不溶性膳食纤维理化特性及其体外酵解对肠道微生物的影响[J]. 食品研究与开发, 2023, 44(24): 23-29, 45.
	LIU D J, ZHOU X Y, WANG F, et al. Physicochemical properties of insoluble dietary fiber from bamboo shoot shells and effects of its in vitro fermentation on intestinal microorganism[J]. Food Research and Development, 2023, 44(24): 23-29, 45. (in Chinese with English abstract)
[15]	沈康, 郭瑞成, 徐天旭, 等. DEAE-52纤维素柱层析纯化处理对西梅可溶性膳食纤维的影响[J]. 食品与发酵工业, 2024, 50(17): 209-217.
	SHEN K, GUO R C, XU T X, et al. Effect of DEAE-52 cellulose column chromatography on soluble dietary fiber of prune[J]. Food and Fermentation Industries, 2024, 50(17): 209-217. (in Chinese with English abstract)
[16]	陈贵婷, 石凯欣, 张珮珮, 等. 不同品种柑橘皮渣膳食纤维构效关系比较[J]. 食品科学, 2023, 44(17): 20-28.
	CHEN G T, SHI K X, ZHANG P P, et al. Comparative study on the structure-activity relationship of dietary fiber from different varieties of Citrus peel and pomace[J]. Food Science, 2023, 44(17): 20-28. (in Chinese with English abstract)
[17]	赵宇楠, 贾丹丹, 蔡丹, 等. 食用菌发酵对人参不溶性膳食纤维结构及功能特性的影响[J]. 食品科学, 2023, 44(22): 80-88.
	ZHAO Y N, JIA D D, CAI D, et al. Effect of edible fungal fermentation on structure and functional properties of ginseng insoluble dietary fiber[J]. Food Science, 2023, 44(22): 80-88. (in Chinese with English abstract)
[18]	张倩, 王佩瑶, 王子成, 等. 碱性过氧化氢处理对藕渣不溶性膳食纤维结构及功能特性的影响[J]. 中国食品学报, 2024, 24(2): 53-61.
	ZHANG Q, WANG P Y, WANG Z C, et al. Effect of alkaline hydrogen peroxide treatment on structure and functional properties of insoluble dietary fiber from lotus root residue[J]. Journal of Chinese Institute of Food Science and Technology, 2024, 24(2): 53-61. (in Chinese with English abstract)
[19]	段振. 石榴皮不溶性膳食纤维的提取、体外降血脂活性研究及咀嚼片制备[D]. 西安: 陕西师范大学, 2018.
	DUAN Z. Extraction of insoluble dietary fiber from pomegranate peel, study on its in vitro lipid-lowering activity, and preparation of chewable tablets[D]. Xi’an: Shaanxi Normal University, 2018. (in Chinese with English abstract)
[20]	池玉闽, 董怡, 何强, 等. 油橄榄果肉和核壳中膳食纤维的功能特性分析[J]. 现代食品科技, 2023, 39(5): 157-163.
	CHI Y M, DONG Y, HE Q, et al. Analysis of the functional properties of dietary fibers from olive pulp and kernel shell[J]. Modern Food Science and Technology, 2023, 39(5): 157-163. (in Chinese with English abstract)
[21]	高一帆, 李若思, 吉莉, 等. 超声波辅助纤维素酶提取黄瓜皮色素工艺研究[J]. 食品研究与开发, 2022, 43(11): 142-147.
	GAO Y F, LI R S, JI L, et al. Study on ultrasonic-assisted cellulase extraction of pigment from cucumber peel[J]. Food Research and Development, 2022, 43(11): 142-147. (in Chinese with English abstract)
[22]	卜智斌, 曾劲, 禹淞文, 等. 超声辅助复合酶法提取马蹄渣不溶性膳食纤维工艺优化及品质对比[J]. 现代食品科技, 2023, 39(7): 177-183.
	BU Z B, ZENG J, YU S W, et al. Process optimization for ultrasound-assisted composite enzymatic extraction of insoluble dietary fiber from water chestnut dregs and quality comparison[J]. Modern Food Science and Technology, 2023, 39(7): 177-183. (in Chinese with English abstract)
[23]	李晗, 杨宗玲, 毕永雪, 等. 超声辅助酶法提取西番莲果皮可溶性膳食纤维及理化性质[J]. 食品工业科技, 2020, 41(7): 161-165.
	LI H, YANG Z L, BI Y X, et al. Extraction of soluble dietary fiber from Passiflora edulis peel by ultrasonic assisted enzymatic method and its physicochemical properties[J]. Science and Technology of Food Industry, 2020, 41(7): 161-165. (in Chinese with English abstract)
[24]	ZHANG S S, XU X L, CAO X, et al. The structural characteristics of dietary fibers from Tremella fuciformis and their hypolipidemic effects in mice[J]. Food Science and Human Wellness, 2023, 12(2): 503-511.
[25]	LIU H F, ZENG X Y, HUANG J Y, et al. Dietary fiber extracted from pomelo fruitlets promotes intestinal functions, both in vitro and in vivo[J]. Carbohydrate Polymers, 2021, 252: 117186.
[26]	何雅静, 陈珊珊, 孙志高. 柑橘皮渣膳食纤维的特性及其在食品中的应用[J]. 食品工业科技, 2021, 42(19): 436-442.
	HE Y J, CHEN S S, SUN Z G. Characteristics of Citrus peel dietary fiber and its application in food[J]. Science and Technology of Food Industry, 2021, 42(19): 436-442. (in Chinese with English abstract)
[27]	王梦阳. 香蕉皮膳食纤维的理化性质及其降血糖效果的研究[D]. 合肥: 合肥工业大学, 2022.
	WANG M Y. Study on the physicochemical properties of banana peel dietary fiber and its hypoglycemic effect[D]. Hefei: Hefei University of Technology, 2022. (in Chinese with English abstract)
[28]	种俸亭, 黄子珍, 滕建文, 等. 百香果皮体外抑制葡萄糖吸收、抗氧化及调节高血糖大鼠肠道菌群结构的作用[J]. 食品科学, 2021, 42(5): 193-200.
	CHONG F T, HUANG Z Z, TENG J W, et al. Antioxidant effect of passion fruit peel and its effect on inhibiting glucose absorption in vitro and regulating intestinal microflora structure in hyperglycemic rats[J]. Food Science, 2021, 42(5): 193-200. (in Chinese with English abstract)
[29]	柏婷梅. 四种麦类膳食纤维结构与体外功能的对比研究[D]. 雅安: 四川农业大学, 2020.
	BAI T M. Comparative study on the structure and in vitro function of dietary fiber from four types of wheat[D]. Ya’an: Sichuan Agricultural University, 2020. (in Chinese with English abstract)
[30]	张馨月, 张民, 邓梅, 等. 三种食物来源膳食纤维的理化性质与功能特性比较[J]. 现代食品科技, 2024, 40(1): 102-111.
	ZHANG X Y, ZHANG M, DENG M, et al. Comparison of the physicochemical properties and functional properties of insoluble dietary fiber from three food sources[J]. Modern Food Science and Technology, 2024, 40(1): 102-111. (in Chinese with English abstract)
[31]	符旭栋. 柠檬皮渣膳食纤维制备及生物改性研究[D]. 重庆: 西南大学, 2022.
	FU X D. Preparation and biomodification of dietary fiber from lemon peel residue[D]. Chongqing: Southwest University, 2022. (in Chinese with English abstract)

Optimization of extraction process for soluble and insoluble dietary fibers from Ougan (Citrus suavissima Hort. ex Tanaka) pomace and the differences between their physicochemical properties and functional characteristics

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