CIESC Journal ›› 2019, Vol. 70 ›› Issue (S1): 124-129.DOI: 10.11949/j.issn.0438-1157.20181483
• Separation engineering • Previous Articles Next Articles
Mixia MA1,2,4(),Ning QIN3,4,Qing MIN3,Wenxiang HU1,4()
Received:
2018-12-17
Revised:
2019-03-02
Online:
2019-03-31
Published:
2019-03-31
Contact:
Wenxiang HU
通讯作者:
胡文祥
作者简介:
<named-content content-type="corresp-name">马密霞</named-content>(1967—),女,博士研究生,副教授,<email>mixia107@163.com</email>|胡文祥(1961—),男,博士,教授,<email>huwx66@163.com</email>
基金资助:
CLC Number:
Mixia MA, Ning QIN, Qing MIN, Wenxiang HU. Resveratrol and polydatin by microwave-ultrasound extraction and determination by HPLC[J]. CIESC Journal, 2019, 70(S1): 124-129.
马密霞, 秦宁, 闵清, 胡文祥. 微波超声波联用萃取白藜芦醇及其苷的HPLC测定[J]. 化工学报, 2019, 70(S1): 124-129.
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URL: https://hgxb.cip.com.cn/EN/10.11949/j.issn.0438-1157.20181483
时间/min | 乙腈/% | 水/% | 流速/ (ml/min) | 梯度类型 |
---|---|---|---|---|
0 7 9 20 | 28 72 72 28 | 72 28 28 72 | 1.0 1.0 1.0 1.0 | 6 6 6 1 |
Table 1 Gradient elution
时间/min | 乙腈/% | 水/% | 流速/ (ml/min) | 梯度类型 |
---|---|---|---|---|
0 7 9 20 | 28 72 72 28 | 72 28 28 72 | 1.0 1.0 1.0 1.0 | 6 6 6 1 |
水平 | 因素 | ||
---|---|---|---|
乙醇浓度(A)/% | 提取时间(B)/min | 提取温度(C)/℃ | |
1 | 40 | 3.0 | 65 |
2 | 50 | 3.5 | 70 |
3 | 60 | 4.0 | 75 |
4 | 70 | 4.5 | 80 |
Table 2 Factors for extraction of resveratrol in peanut buds
水平 | 因素 | ||
---|---|---|---|
乙醇浓度(A)/% | 提取时间(B)/min | 提取温度(C)/℃ | |
1 | 40 | 3.0 | 65 |
2 | 50 | 3.5 | 70 |
3 | 60 | 4.0 | 75 |
4 | 70 | 4.5 | 80 |
实验号 | 因素 | 浸膏质量/g | 浸膏得率/% | 浸膏得率评分 | 白藜芦醇含量/% | 白藜芦醇含量评分 | 综合评分 | ||
---|---|---|---|---|---|---|---|---|---|
A | B | C | |||||||
1 | 1 | 1 | 1 | 0.90 | 30.00 | 22.64 | 0.4977 | 60.00 | 82.64 |
2 | 1 | 2 | 2 | 1.59 | 53.00 | 40.00 | 0.2932 | 35.35 | 75.35 |
3 | 1 | 3 | 3 | 0.76 | 25.33 | 19.12 | 0.2819 | 33.98 | 53.10 |
4 | 1 | 4 | 4 | 0.97 | 32.33 | 24.40 | 0.0378 | 4.56 | 28.96 |
5 | 2 | 1 | 2 | 0.87 | 29.00 | 21.89 | 0.0328 | 3.95 | 25.84 |
6 | 2 | 2 | 1 | 0.80 | 26.67 | 20.13 | 0.0225 | 2.71 | 22.84 |
7 | 2 | 3 | 4 | 1.25 | 41.67 | 31.45 | 0.0348 | 4.20 | 35.64 |
8 | 2 | 4 | 3 | 1.26 | 42.00 | 31.70 | 0.0076 | 0.92 | 32.61 |
9 | 3 | 1 | 3 | 1.33 | 44.33 | 33.46 | 0.0259 | 3.12 | 36.58 |
10 | 3 | 2 | 4 | 1.12 | 37.33 | 28.18 | 0.0060 | 0.72 | 28.90 |
11 | 3 | 3 | 1 | 1.03 | 34.33 | 25.91 | 0.0486 | 5.86 | 31.77 |
12 | 3 | 4 | 2 | 1.00 | 33.33 | 25.16 | 0.0247 | 2.98 | 28.13 |
13 | 4 | 1 | 4 | 1.06 | 35.33 | 26.67 | 0.0281 | 3.39 | 30.05 |
14 | 4 | 2 | 3 | 0.68 | 22.67 | 17.11 | 0.0900 | 10.85 | 27.96 |
15 | 4 | 3 | 2 | 0.97 | 32.33 | 24.40 | 0.0193 | 2.33 | 26.73 |
16 | 4 | 4 | 1 | 0.95 | 31.67 | 23.90 | 0.0860 | 10.37 | 34.27 |
K1 | 60.01 | 43.78 | 42.88 | ||||||
K2 | 29.23 | 38.76 | 22.29 | ||||||
K3 | 31.35 | 36.81 | 37.56 | ||||||
K4 | 29.75 | 30.99 | 30.89 | ||||||
R | 0.78 | 12.79 | 20.59 |
Table 3 Orthogonal test results of resveratrol extraction from peanut buds
实验号 | 因素 | 浸膏质量/g | 浸膏得率/% | 浸膏得率评分 | 白藜芦醇含量/% | 白藜芦醇含量评分 | 综合评分 | ||
---|---|---|---|---|---|---|---|---|---|
A | B | C | |||||||
1 | 1 | 1 | 1 | 0.90 | 30.00 | 22.64 | 0.4977 | 60.00 | 82.64 |
2 | 1 | 2 | 2 | 1.59 | 53.00 | 40.00 | 0.2932 | 35.35 | 75.35 |
3 | 1 | 3 | 3 | 0.76 | 25.33 | 19.12 | 0.2819 | 33.98 | 53.10 |
4 | 1 | 4 | 4 | 0.97 | 32.33 | 24.40 | 0.0378 | 4.56 | 28.96 |
5 | 2 | 1 | 2 | 0.87 | 29.00 | 21.89 | 0.0328 | 3.95 | 25.84 |
6 | 2 | 2 | 1 | 0.80 | 26.67 | 20.13 | 0.0225 | 2.71 | 22.84 |
7 | 2 | 3 | 4 | 1.25 | 41.67 | 31.45 | 0.0348 | 4.20 | 35.64 |
8 | 2 | 4 | 3 | 1.26 | 42.00 | 31.70 | 0.0076 | 0.92 | 32.61 |
9 | 3 | 1 | 3 | 1.33 | 44.33 | 33.46 | 0.0259 | 3.12 | 36.58 |
10 | 3 | 2 | 4 | 1.12 | 37.33 | 28.18 | 0.0060 | 0.72 | 28.90 |
11 | 3 | 3 | 1 | 1.03 | 34.33 | 25.91 | 0.0486 | 5.86 | 31.77 |
12 | 3 | 4 | 2 | 1.00 | 33.33 | 25.16 | 0.0247 | 2.98 | 28.13 |
13 | 4 | 1 | 4 | 1.06 | 35.33 | 26.67 | 0.0281 | 3.39 | 30.05 |
14 | 4 | 2 | 3 | 0.68 | 22.67 | 17.11 | 0.0900 | 10.85 | 27.96 |
15 | 4 | 3 | 2 | 0.97 | 32.33 | 24.40 | 0.0193 | 2.33 | 26.73 |
16 | 4 | 4 | 1 | 0.95 | 31.67 | 23.90 | 0.0860 | 10.37 | 34.27 |
K1 | 60.01 | 43.78 | 42.88 | ||||||
K2 | 29.23 | 38.76 | 22.29 | ||||||
K3 | 31.35 | 36.81 | 37.56 | ||||||
K4 | 29.75 | 30.99 | 30.89 | ||||||
R | 0.78 | 12.79 | 20.59 |
产物 | 峰面积 | 平均值 | RSD/% | |||||
---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | |||
白藜芦醇 | 3638.987 | 3672.407 | 3682.220 | 3647.186 | 3584.484 | 3652.530 | 3646.302 | 0.94 |
白藜芦醇苷 | 113.618 | 112.469 | 114.125 | 110.829 | 112.542 | 112.634 | 112.703 | 0.92 |
Table 4 Precision experiment
产物 | 峰面积 | 平均值 | RSD/% | |||||
---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | |||
白藜芦醇 | 3638.987 | 3672.407 | 3682.220 | 3647.186 | 3584.484 | 3652.530 | 3646.302 | 0.94 |
白藜芦醇苷 | 113.618 | 112.469 | 114.125 | 110.829 | 112.542 | 112.634 | 112.703 | 0.92 |
产物 | 峰面积 | 平均值 | RSD/% | |||||
---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | |||
白藜芦醇 | 192.127 | 194.273 | 188.896 | 190.485 | 193.562 | 189.500 | 191.640 | 0.95 |
白藜芦醇苷 | 587.326 | 587.926 | 593.455 | 592.783 | 586.344 | 574.787 | 587.100 | 1.04 |
Table 5 Repeated experiment
产物 | 峰面积 | 平均值 | RSD/% | |||||
---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | |||
白藜芦醇 | 192.127 | 194.273 | 188.896 | 190.485 | 193.562 | 189.500 | 191.640 | 0.95 |
白藜芦醇苷 | 587.326 | 587.926 | 593.455 | 592.783 | 586.344 | 574.787 | 587.100 | 1.04 |
花生芽 | 葡萄籽 | |||||||
---|---|---|---|---|---|---|---|---|
样品号 | 白藜芦醇含量/% | 平均值/% | 白藜芦醇苷含量/% | 平均值/% | 白藜芦醇含量/% | 平均值/% | 白藜芦醇苷含量/% | 平均值/% |
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 | 0.4977 0.2932 0.2819 0.0378 0.0328 0.0225 0.0348 0.0076 0.0259 0.0060 0.0486 0.0247 0.0281 0.0900 0.0193 0.0965 | 0.0967 | 0.1186 0.1153 0.0039 0.0260 0.0340 0.0239 0.0491 0.0213 0.0358 0.0092 0.0856 0.0988 0.0537 0.0913 0.0091 0.0509 | 0.0519 | 2.529 3.187 2.306 0.756 1.859 0.720 1.204 2.091 1.568 2.128 2.334 1.121 1.955 1.232 2.164 1.799 | 1.810 | 2.609 2.032 1.998 1.987 1.159 1.972 0.969 1.248 1.987 2.264 2.026 1.953 1.943 1.987 1.029 1.872 | 1.811 |
Table 6 Results of resveratrol content determination
花生芽 | 葡萄籽 | |||||||
---|---|---|---|---|---|---|---|---|
样品号 | 白藜芦醇含量/% | 平均值/% | 白藜芦醇苷含量/% | 平均值/% | 白藜芦醇含量/% | 平均值/% | 白藜芦醇苷含量/% | 平均值/% |
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 | 0.4977 0.2932 0.2819 0.0378 0.0328 0.0225 0.0348 0.0076 0.0259 0.0060 0.0486 0.0247 0.0281 0.0900 0.0193 0.0965 | 0.0967 | 0.1186 0.1153 0.0039 0.0260 0.0340 0.0239 0.0491 0.0213 0.0358 0.0092 0.0856 0.0988 0.0537 0.0913 0.0091 0.0509 | 0.0519 | 2.529 3.187 2.306 0.756 1.859 0.720 1.204 2.091 1.568 2.128 2.334 1.121 1.955 1.232 2.164 1.799 | 1.810 | 2.609 2.032 1.998 1.987 1.159 1.972 0.969 1.248 1.987 2.264 2.026 1.953 1.943 1.987 1.029 1.872 | 1.811 |
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