固相萃取-高效液相色谱法测定植物源性产品中的熊果苷

doi:10.3969/j.issn.1004-1524.20240448

浙江农业学报 ›› 2025, Vol. 37 ›› Issue (8): 1776-1784.DOI: 10.3969/j.issn.1004-1524.20240448

固相萃取-高效液相色谱法测定植物源性产品中的熊果苷

陈敏¹^,²(), 张巧艳², 王夏君², 王顺利¹^,^*(), 郑蔚然²^,^*()

1.浙江理工大学理学院,浙江杭州 310018
2.浙江省农业科学院农产品质量安全与营养研究所,浙江杭州 310021

收稿日期:2024-05-22 出版日期:2025-08-25 发布日期:2025-09-03
作者简介:陈敏(1999—),男,江西赣州人,硕士,研究方向为农产品质量安全。E-mail: 1828010594@qq.com
通讯作者: *王顺利,E-mail: slwang@zstu.edu.cn;郑蔚然,E-mail: rancki@163.com
基金资助:
农业行业标准制修订项目(2019R19A24C10);现代农业产业技术体系建设专项(CARS-29)

Determination of arbutin in plant-derived products by solid phase extraction-high performance liquid chromatography

CHEN Min¹^,²(), ZHANG Qiaoyan², WANG Xiajun², WANG Shunli¹^,^*(), ZHENG Weiran²^,^*()

1. School of Science, Zhejiang Sci-Tech University, Hangzhou 310018, China
2. Institute of Agro-product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2024-05-22 Online:2025-08-25 Published:2025-09-03
Contact: WANG Shunli,ZHENG Weiran

摘要/Abstract

摘要： 建立了测定植物源性产品(水果与中草药)中熊果苷的固相萃取-高效液相色谱法,分别采用水与甲醇对高含水量样品和低含水量样品进行提取,通过HLB固相萃取小柱净化,利用高效液相色谱进行测定。结果表明:在0.000 5~0.05 mg·mL^-1范围内,熊果苷质量浓度与色谱峰峰面积具有良好的线性关系,相关系数为0.999 8,3个不同加标水平下熊果苷的回收率为81.33%~97.01%,相对标准偏差为1.39%~3.65%(n=6)。将建立的方法应用于植物源性产品检测,发现梨的熊果苷含量较高,蓝莓、覆盆子及白及次之。该方法实用性强、结果准确、适用范围广,可作为植物源性产品中熊果苷的检测方法,为植物源性产品的品质评估提供科学参考。

关键词: 熊果苷, 植物源产品, 固相萃取, 高效液相色谱法

Abstract:

A solid phase extraction(SPE)-high performance liquid chromatography (HPLC) method was developed for the determination of arbutin in plant-derived products ( fruits and Chinese herbal medicines). The samples with high water content and low water content were extracted by water and methanol respectively, purified by HLB solid phase extraction column, and analyzed by high performance liquid chromatography. The results showed that the mass concentration of arbutin had a good linear relationship with the chromatographic peak area in the range of 0.000 5-0.05 mg·mL^-1, the correlation coefficient was 0.999 8. The recovery rates of arbutin at three different spiked levels were 81.33%-97.01%, and the relative standard deviations were 1.39%-3.65% (n=6). The established method was applied to plant-derived products. The content of arbutin in pear was higher, followed by blueberry, raspberry and Bletilla striata. The method has good practicability, accurate results and wide application range. It can be used as a detection method for arbutin in plant-derived products and provide scientific reference for the quality evaluation of plant-derived products.

Key words: arbutin, plant-derived product, solid-phase extraction(SPE), high performance liquid chromatography (HPLC)

中图分类号:

陈敏, 张巧艳, 王夏君, 王顺利, 郑蔚然. 固相萃取-高效液相色谱法测定植物源性产品中的熊果苷[J]. 浙江农业学报, 2025, 37(8): 1776-1784.

CHEN Min, ZHANG Qiaoyan, WANG Xiajun, WANG Shunli, ZHENG Weiran. Determination of arbutin in plant-derived products by solid phase extraction-high performance liquid chromatography[J]. Acta Agriculturae Zhejiangensis, 2025, 37(8): 1776-1784.

图/表 8

参考文献 22

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样品 Sample	加标含量 Added content/ (mg·kg^-1)	回收率 Recovery rate/%						平均回收率 Average recoveries/%	RSD/%
样品 Sample	加标含量 Added content/ (mg·kg^-1)	1	2	3	4	5	6	平均回收率 Average recoveries/%	RSD/%
早酥梨	1	83.27	87.15	89.84	84.19	86.76	82.01	85.54	3.39
Zaosu pear	10	88.51	88.05	83.97	84.12	87.78	85.74	86.36	2.35
	100	93.43	96.13	96.07	95.33	94.27	97.01	95.37	1.39
白及	1	81.33	85.48	82.89	89.12	87.65	82.55	84.84	3.65
Bletilla striata	10	86.17	86.14	84.78	82.22	89.75	82.59	85.28	3.29
	100	92.15	93.86	89.44	91.36	94.84	93.15	92.47	2.08

样品 Sample	加标含量 Added content/ (mg·kg^-1)	回收率 Recovery rate/%						平均回收率 Average recoveries/%	RSD/%
样品 Sample	加标含量 Added content/ (mg·kg^-1)	1	2	3	4	5	6	平均回收率 Average recoveries/%	RSD/%
早酥梨	1	83.27	87.15	89.84	84.19	86.76	82.01	85.54	3.39
Zaosu pear	10	88.51	88.05	83.97	84.12	87.78	85.74	86.36	2.35
	100	93.43	96.13	96.07	95.33	94.27	97.01	95.37	1.39
白及	1	81.33	85.48	82.89	89.12	87.65	82.55	84.84	3.65
Bletilla striata	10	86.17	86.14	84.78	82.22	89.75	82.59	85.28	3.29
	100	92.15	93.86	89.44	91.36	94.84	93.15	92.47	2.08

样品 Sample	称样量 Sample weight/g	提取溶剂 Extraction solvent	提取溶剂体积 Extraction solvent volume/mL	超声时间 Ultrasonic time/min	固相萃取柱 Solid phase extraction	含量 Content/ (mg·kg^-1)	文献 Reference
覆盆子Raspberry	1.00	甲醇Methanol	4	30	HLB	12.92	本文This study
覆盆子Raspberry	1.00	水Water	10	30	无None	ND	[18]
覆盆子Raspberry	1.00	水Water	100	30	无None	ND	[13]
覆盆子Raspberry	1.00	70%甲醇70% Methanol	150	30	HLB	ND	[20]
覆盆子Raspberry	1.00	70%甲醇70% Methanol	50	30	HLB	11.54	[21]
早酥梨Zaosu pear	1.00	水Water	4	20	HLB	87.69	本文This study
早酥梨Zaosu pear	1.00	乙醇Ethanol	4	0	C18	19.69	[15]
早酥梨Zaosu pear	1.00	80%甲醇80% Methanol	10	0	无None	76.85	[22]

样品 Sample	称样量 Sample weight/g	提取溶剂 Extraction solvent	提取溶剂体积 Extraction solvent volume/mL	超声时间 Ultrasonic time/min	固相萃取柱 Solid phase extraction	含量 Content/ (mg·kg^-1)	文献 Reference
覆盆子Raspberry	1.00	甲醇Methanol	4	30	HLB	12.92	本文This study
覆盆子Raspberry	1.00	水Water	10	30	无None	ND	[18]
覆盆子Raspberry	1.00	水Water	100	30	无None	ND	[13]
覆盆子Raspberry	1.00	70%甲醇70% Methanol	150	30	HLB	ND	[20]
覆盆子Raspberry	1.00	70%甲醇70% Methanol	50	30	HLB	11.54	[21]
早酥梨Zaosu pear	1.00	水Water	4	20	HLB	87.69	本文This study
早酥梨Zaosu pear	1.00	乙醇Ethanol	4	0	C18	19.69	[15]
早酥梨Zaosu pear	1.00	80%甲醇80% Methanol	10	0	无None	76.85	[22]

水果Fruit	含量Content/(mg·kg^-1)	中草药Chinese herbal medicine	含量Content/(mg·kg^-1)
苹果Apple	ND	元胡Corydalis yanhusuo	ND
脐橙Navel orange	ND	玄参Scrophularia yunnanensis	ND
葡萄Grape	ND	浙贝母Fritillaria thunbergii	ND
水蜜桃Peach	ND	白芍Paeonia lactiflora	ND
草莓Strawberry	ND	白术Atractylodes macrocephala	ND
石榴Pomegranate	ND	覆盆子Raspberry	12.92
红果参Campanumoea lancifolia	ND	白及Bletilla striata	8.13
早酥梨Zaosu pear	87.69	黄芩Scutellaria baicalensis	ND
蓝莓Blueberry	13.39	铁皮石斛Dendrobium officinale	3.25

固相萃取-高效液相色谱法测定植物源性产品中的熊果苷

Determination of arbutin in plant-derived products by solid phase extraction-high performance liquid chromatography

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t/min	A/%	B/%	流速Flow rate/(mL·min^-1)
0	95	5	0.8
12	95	5	0.8
15	70	30	0.8
17	20	80	0.8
20	95	5	0.8
23	95	5	0.8

t/min	A/%	B/%	流速Flow rate/(mL·min^-1)
0	95	5	0.8
12	95	5	0.8
15	70	30	0.8
17	20	80	0.8
20	95	5	0.8
23	95	5	0.8