Macroporous Resin Purifying Polyphenols from Empetrum nigrum Aerial Parts

doi:10.7525/j.issn.1673-5102.2021.04.018

Abstract

Abstract:

In order to optimize the process of polyphenols by macroporous resin from Empetrum nigrum aerial parts， moisture content， adsorption rate and desorption rate of six resins（HPD-100， X-5， AB-8， D101， HPD-600 and NKA-Ⅱ） were investigated， and the resin with the best effect was selected. Four factors（sample concentration， ethanol concentration， elution flow rate and elution volume） that have a great influence on the purification process were selected， and the response surface method was used to analyze the optimal process. HPD-600 macroporous resin had the best purification effect on polyphenols yield. The optimal extraction conditions were as follows： sample concentration was 0.84 mg·mL^-1， ethanol concentration was 62.15%， elution flow rate was 0.67 mL·min^-1， and elution volume was 2.71 BV. Under these conditions， the yield of polyphenols was 229.18 mg·g^-1， the purity of polyphenols was increased from 8.11% to 22.56%， and the recovery rate was 67.78%.

Key words: Empetrum nigrum, polyphenols, macroporous resin, response surface method, purification process

CLC Number:

S567.9

Yuan GAO, Wen-Xin XING, Hui-Mei WANG. Macroporous Resin Purifying Polyphenols from Empetrum nigrum Aerial Parts[J]. Bulletin of Botanical Research, 2021, 41(4): 626-632.

Figures/Tables 7

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类型 Trade name	极性 Polarity	比表面积 Surface area (m²g)	平均孔径 Average pore diameter(nm)	粒径范围Particle diameter (mm)
HPD-100	非极性Nonpolarity	650~700	9~10	0.3~1.25
X-5	非极性Nonpolarity	500~600	29~30	0.25~0.84
AB-8	弱极性Weak polarity	480~520	13~14	0.3~1.25
D101	弱极性Weak polarity	500~550	9~10	0.25~0.84
HPD-600	极性Polarity	550~600	8	0.30~1.20
NKA-Ⅱ	极性Polarity	160~200	14.5~15.5	0.30~1.25

类型 Trade name	含水率 Moisture content (%)	吸附率 Adsorption rate (%)	解吸率 Desorption rate (%)
HPD-100	61.16±0.77	55.95±0.46	74.56±0.82
X-5	71.94±0.84	56.98±0.66	53.81±0.54
AB-8	73.27±0.28	62.93±0.84	23.75±0.98
D101	73.06±0.34	64.11±0.72	29.60±0.62
HPD-600	76.74±0.56	72.49±0.55	77.25±0.47
NKA-Ⅱ	59.40±0.58	58.84±1.12	25.40±0.71

序号 No.	A:上样浓度 Sample concentration (mg·mL^-1)	B:乙醇浓度 Ethanol concentration (%)	C:洗脱流速 Elution flow rate (mL·min^-1)	D:洗脱体积 Elution volume (BV)	提取率 Extraction yield (mg·g^-1)
1	0.80	70.00	0.50	1.00	68.85
2	0.60	70.00	1.00	1.00	72.92
3	0.80	60.00	0.50	2.00	168.24
4	0.80	80.00	1.00	3.00	180.26
5	0.80	60.00	1.00	3.00	211.00
6	0.80	80.00	0.50	2.00	175.51
7	0.80	70.00	1.00	2.00	212.12
8	0.80	60.00	1.00	1.00	77.67
9	0.80	70.00	1.00	2.00	200.94
10	0.60	80.00	1.00	2.00	87.01
11	0.80	70.00	0.50	3.00	224.69
12	0.80	70.00	1.00	2.00	195.63
13	1.00	80.00	1.00	2.00	165.72
14	1.00	70.00	1.00	1.00	94.56
15	0.80	60.00	1.50	2.00	129.67
16	0.80	80.00	1.50	2.00	186.40
17	1.00	70.00	1.50	2.00	199.26
18	0.80	80.00	1.00	1.00	61.02
19	0.80	70.00	1.00	2.00	216.31
20	0.60	60.00	1.00	2.00	101.05
21	1.00	60.00	1.00	2.00	174.95
22	1.00	70.00	0.50	2.00	211.28
23	0.60	70.00	1.00	3.00	155.66
24	1.00	70.00	1.00	3.00	216.31
25	0.60	70.00	0.50	2.00	125.30
26	0.80	70.00	1.50	3.00	175.51
27	0.80	70.00	1.00	2.00	224.13
28	0.60	70.00	1.50	2.00	74.37
29	0.80	70.00	1.50	1.00	86.79

来源 Source	平方和 Sum of squares	自由度 df	均方 Mean square	F值 F-value	P值 P-value	显著性 Significance
模型Model	82 747.21	14	5 910.51	14.61	<0.000 1	??
A	16 559.24	1	16 559.24	40.92	<0.000 1	??
B	3.70	1	3.70	9.135E-003	0.925 2
C	1 237.69	1	1 237.69	3.06	0.102 2
D	41 022.55	1	41 022.55	101.38	< 0.000 1	??
AB	5.78	1	5.78	0.014	0.906 5
AC	378.50	1	378.50	0.94	0.349 9
AD	380.45	1	380.45	0.94	0.348 7
BC	611.57	1	611.57	1.51	0.239 2
BD	49.63	1	49.63	0.12	0.731 4
CD	1 126.27	1	1 126.27	2.78	0.117 4
A²	9 258.80	1	9 258.80	22.88	0.000 3	??
B²	6 964.46	1	6 964.46	17.21	0.001 0	??
C²	2 427.66	1	2 427.66	6.00	0.028 1	?
D²	12 801.41	1	12 801.41	31.64	< 0.000 1	??
残差Residual	5 665.00	14	404.64
失拟项Lack of fit	5 132.61	10	513.26	3.86	0.102 6
纯误差Pure error	532.40	4	133.10
总变异Cor total	88 412.21	28
R²	0.935 9		R²_Adj	0.871 9

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