微波超声波联用萃取白藜芦醇及其苷的HPLC测定

doi:10.11949/j.issn.0438-1157.20181483

化工学报 ›› 2019, Vol. 70 ›› Issue (S1): 124-129.DOI: 10.11949/j.issn.0438-1157.20181483

微波超声波联用萃取白藜芦醇及其苷的HPLC测定

马密霞^1,^2,⁴(),秦宁^3,⁴,闵清³,胡文祥^1,⁴()

1. 武汉工程大学化学与环境工程学院, 湖北武汉 430073
2. 北京联合大学智慧城市学院, 北京 100101
3. 湖北科技学院药学院, 湖北咸宁 437100
4. 北京神剑天军医学科学院京东祥鹄微波化学联合实验室, 北京 101601

收稿日期:2018-12-17 修回日期:2019-03-02 出版日期:2019-03-31 发布日期:2019-03-31
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:
北京市创新基金项目(Z080104024508111)

Resveratrol and polydatin by microwave-ultrasound extraction and determination by HPLC

Mixia MA^1,^2,⁴(),Ning QIN^3,⁴,Qing MIN³,Wenxiang HU^1,⁴()

1. School of Chemical and Environmental Engineering, Wuhan Institute of Technology, Wuhan 430073, Hubei, China
2. Smart City College, Beijing Union University, Beijing 100101, China
3. School of Pharmacy, Hubei University of Science and Technology, Xianning 437100, Hubei, China
4. Jingdong Xianghu Microwave Chemistry Union Laboratory, Beijing Excalibur Space Military Academy of Medical Sciences, Beijing 101601, China

Received:2018-12-17 Revised:2019-03-02 Online:2019-03-31 Published:2019-03-31
Contact: Wenxiang HU

摘要/Abstract

摘要：

建立了花生芽和葡萄籽微波超声波联用提取白黎芦醇及其苷的HPLC测定方法。采用高效液相色谱进行测定,色谱柱为迪马C₁₈, 流动相为乙腈-水溶液，梯度洗脱，流速1.0 ml/min，柱温为30℃，检测波长为306 nm，进样量为20 μl。白黎芦醇在0.343～15.15×10³ μg/ml范围内呈良好的线性关系，相关系数R² = 0.9967；白藜芦醇苷在110.712～1774.23×10³ μg /ml范围内线性关系良好，相关系数R² = 0.9993。该方法检测快速、简便、重现性好，适用于花生芽和葡萄籽中白藜芦醇及其苷的定量分析。

关键词: 微波超声波, 萃取, 白藜芦醇, 药物, 色谱, 浸取

Abstract:

Objective to establish a method for the determination of resveratrol and polydatin in peanut bud and grape pip extract. High performance liquid chromatography (HPLC) was used. The chromatographic column was Di Ma C₁₈, the mobile phase was acetonitrile water solution, gradient elution, flow rate 1 ml/min, column temperature 30℃, 306 nm and 20 μl. The linear range of resveratol showed good linear relationship 0.343－15.15×10³μg /ml, R² = 0.9967. The linear range of polydatin showed good linear relationship 110.712－1774.23×10³ μg/ml, R² = 0.9993. The method is rapid, simple and reproducible, and is suitable for quantitative analysis of resveratrol in peanut sprouts and grape seeds.

Key words: microwave ultrasonic wave, extraction, resveratrol, pharmaceuticals, chromatography, leaching

中图分类号:

R 284

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.

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.

图/表 6

参考文献 31

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水平	因素
水平	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

水平	因素
水平	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
实验号	A	B	C	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
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

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
实验号	A	B	C	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
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/%
产物	1	2	3	4	5	6	平均值	RSD/%
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

微波超声波联用萃取白藜芦醇及其苷的HPLC测定

Resveratrol and polydatin by microwave-ultrasound extraction and determination by HPLC

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产物	峰面积						平均值	RSD/%
产物	1	2	3	4	5	6	平均值	RSD/%
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

产物	峰面积						平均值	RSD/%
产物	1	2	3	4	5	6	平均值	RSD/%
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