纳滤法制备高纯度雪莲果低聚果糖及其结构表征

doi:10.3969/j.issn.1673-5854.2020.05.006

Abstract

Abstract:

The yacon fructo-oligosaccharides(FOS) was separated and purified by the nanometer membrane from yacon. A quadratic mathematical model for predioting the concentration of oligosaccharides was developed to optimize the purification process by Box-Behnken central composite design(CCD) and response surface methodology(RSM). Consequently, the optimized processing parameters were determined as operating pressure 0.15 MPa, circulation flow rate 5.3 mL/min, pH value 2.7, purification fold 5, the purity of the obtained FOS was 95.1%, which could reach P grade standard. HPLC-MS, IR, ¹H NMR and ¹³C NMR were used to characterize the purity, composition and structure of FOS. The results showed that the purified FOS was composed of kestose, nystose and bestonentaose. The purity was 95.1% and it contained on average of 5 fructose units. The yacon FOS was mainly composed of β-furan-fructose tested by IR.

Key words: yacon, FOS, nanofiltration, separation and purification, structure characterization

CLC Number:

TQ35

Xiaomeng QU,Ge YANG,Zehao ZHANG,Lan ZHANG. Preparation of High Purity Yacon Fructo-oligosaccharides by Nanofiltration and Its Characterization[J]. Biomass Chemical Engineering, 2020, 54(5): 37-44.

Figures/Tables 12

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References 25

1	PROSKY L , HOEBREGS H . Methods to determine food inulin and oligo-fructose[J]. The Journal of Nutrition, 1999, 129, 1418S- 1423S. doi: 10.1093/jn/129.7.1418S
2	GRAEFE S , HERMANN M , MANRIQUE I , et al. Effects of post-harvest treatments on thecarbohydrate composition ofyacon roots in the Peruvian Andes[J]. Field Crops Research, 2004, 86 (2/3): 157- 165.
3	SIMONOVSKA B , VOVK I , ANDRENŠEK S , et al. Investigation of phenolic acids in yacon(Smallanthus sonchifolius)leaves and tubers[J]. Journal of Chro-matography A, 2003, 1016, 89- 98. doi: 10.1016/S0021-9673(03)01183-X
4	郑金利. 亚贡引种观察及栽培技术[J]. 北方果树, 2005, (2): 32- 33.
5	KELLY-QUAGLIANA K A , NELSON P D , BUDDINGTON R K . Dietary oligofructose and inulin modulate immune functions in mice[J]. Nutrition Research, 2003, 23 (2): 257- 267. doi: 10.1016/S0271-5317(02)00516-X
6	SCHORR K , DA COSTA F B . Quantitative determination of enhydrin in leaf rinse extracts and in glandular trichomes of Smallanthus sonchifolius(Asteraceae) by reversed-phase high-performance liquid chromatography[J]. Phytochemical Analysis, 2005, 16 (3): 161- 165. doi: 10.1002/pca.836
7	TAKENAKA M , YAN X J , ONO H , et al. Caffeic acid derivatives in the roots of yacon(Smallanthus sonchifolius)[J]. Journal of Agricultural and Food Chemistry, 2003, 51 (3): 793- 796. doi: 10.1021/jf020735i
8	韩永, 林强, 王晓琳. 低聚壳聚糖制备液纳滤纯化的可行性研究[J]. 离子交换与吸附, 2012, 28 (1): 86- 91.
9	江波, 王璋. 双酶法生产高纯度低聚果糖的研究[J]. 食品科学, 1997, 18 (9): 24- 27.
10	钱林, 丁长河, 李里特, 等. 雪莲果的化学组分及其功能特性[J]. 食品研究与开发, 2006, 27 (6): 179- 180, 188.
11	李卓亚. 雪莲果化学成分及其药理作用的研究进展[J]. 食品与药品, 2007, 9 (6): 41- 45.
12	饶之坤, 封良燕, 张虽拴. 雪莲果营养成分分析研究[J]. 云南化工, 2007, 34 (1): 53- 55.
13	马莺. 低聚果糖的定性分析[J]. 分析化学, 2002, 30 (5): 635- 638.
14	陈欢欢, 赵峡, 栾晓红, 等. 电喷雾质谱在寡糖序列分析中的应用[J]. 高等学校化学学报, 2015, 36 (1): 1- 8.
15	冯文亮, 王静, 贾晓江. 纳滤技术生产高纯度低聚果糖的研究[J]. 乳业科学与技木, 2003, 26 (3): 102- 105.
16	王湛. 膜分离技术基础[M]. 北京: 化学工业出版社, 2000.
17	刘家祺, 姜忠义, 王春艳. 分离过程与技术[M]. 天津: 天津大学出版社, 2001: 254- 262.
18	罗利华.有机溶液的纳滤过程[D].南京:南京工业大学, 2003.
19	孙蔚榕, 韩亮, 鲍元兴. 低聚糖的纳滤分离技术[J]. 无锡轻工大学学报, 2002, 21 (6): 574- 578, 596.
20	熊蓉春, 雷晓东, 魏刚. γ-Al₂O₃纳滤膜的特性参数及工作曲线[J]. 科学通报, 2003, 48 (7): 5- 7.
21	傅博强, 谢明勇, 周鹏. 茶叶多糖的提取纯化、组成及药理作用研究进展[J]. 南昌大学学报(理科版), 2001, 25 (4): 358- 364.
22	刘萍, 王红斌, 李桂镇, 等. 响应面法优化咖啡壳基高性能活性炭活化条件的研究[J]. 生物质化学工程, 2017, 51 (2): 43- 47.
23	陈颖. 试验设计[M]. 北京: 中国统计出版社, 2004.
24	郝林华, 陈磊. 牛蒡寡糖的分离纯化及结构研究[J]. 高等学校化学学报, 2005, 26 (7): 1242- 1247.
25	田媛, 张尊建. 糖类结构的核磁共振波谱及质谱分析[J]. 药学进展, 2003, 27 (2): 78- 80.

编号 No.	X₁ 操作压力/MPa operation Pressure	X₂ pH值 pH value	X₃ 循环流量(mL/min) circulation flow	X₄ 纯化倍数 purification factor	Y 低聚果糖纯度/% oligofructose concentration
1	0.6	2	7	4	89.8
2	0.1	1	7	4	80.1
3	1.1	2	10	4	89.9
4	0.1	2	10	4	76.8
5	1.1	2	7	6	89.7
6	0.1	2	4	4	88.6
7	0.6	3	7	6	96.2
8	0.1	2	7	6	91.3
9	0.6	2	7	4	90.8
10	0.6	3	10	4	93.6
11	0.6	2	7	4	90.8
12	0.6	3	7	2	82.7
13	0.1	3	7	4	84.6
14	0.6	2	4	6	95.9
15	0.6	1	7	6	90
16	0.6	2	10	6	92.2
17	0.1	2	10	6	84.9
18	0.6	2	7	2	82.5
19	0.6	2	7	4	90.1
20	0.6	1	4	2	83.5
21	0.6	1	4	4	92.3
22	0.6	2	10	4	87.5
23	1.1	2	10	2	85.1
24	1.1	2	4	4	85.9
25	1.1	3	7	4	90.2
26	1.1	1	7	4	83.1
27	0.6	2	7	4	89.8
28	0.6	1	7	2	78.7
29	0.6	3	4	4	80.9

方差来源 source of variance	平方和 SS	自由度 df	均方 MS	F值 F value	P值 P value
模型model	691.30	14	49.38	51.84	< 0.0001
X₁	48.18	1	48.18	50.58	< 0.0001
X₂	63.29	1	63.29	66.45	< 0.0001
X₃	20.50	1	20.50	21.52	0.0004
X₄	376.54	1	376.54	395.31	< 0.0001
X₁X₂	1.69	1	1.69	1.77	0.2041
X₁X₃	70.48	1	70.48	73.99	< 0.0001
X₁X₄	23.36	1	23.36	24.53	0.0002
X₂X₃	154.90	1	154.90	162.62	< 0.0001
X₂X₄	0.54	1	0.54	0.56	0.4658
X₃X₄	1.07	1	1.07	1.12	0.3069
X₁²	75.44	1	75.44	79.20	< 0.0001
X₂²	36.26	1	36.26	38.07	< 0.0001
X₃²	20.84	1	20.84	21.88	0.0004
X₄²	11.96	1	11.96	12.56	0.0032
残差residual	13.34	14	0.95
失拟项lack of fit	12.30	10	1.23	4.77	0.0728
纯误差pure error	1.03	4	0.26
总和sum	704.64	28
决定系数determination coefficient	0.9811
修正系数correction factor	0.9622

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Preparation of High Purity Yacon Fructo-oligosaccharides by Nanofiltration and Its Characterization

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