固相萃取-液相色谱-串联质谱法同时测定蜂蜜中16种黄酮类化合物和阿魏酸

引用本文: 侯建波, 谢文, 钱艳, 史颖珠, 陆顺, 盛涛, 陈文彬. 固相萃取-液相色谱-串联质谱法同时测定蜂蜜中16种黄酮类化合物和阿魏酸[J]. 色谱, 2020, 38(5): 529-537. doi: 10.3724/SP.J.1123.2019.06030 shu

Citation: HOU Jianbo, XIE Wen, QIAN Yan, SHI Yingzhu, LU Shun, SHENG Tao, CHEN Wenbin. Simultaneous determination of 16 flavonoids and ferulic acid in honey by solid phase extraction and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(5): 529-537. doi: 10.3724/SP.J.1123.2019.06030 shu

固相萃取-液相色谱-串联质谱法同时测定蜂蜜中16种黄酮类化合物和阿魏酸

侯建波 ^{1,2,
,} ,
谢文 ^1,2, ,
钱艳 ^3, ,
史颖珠 ^3, ,
陆顺 ^3, ,
盛涛 ^3, ,
陈文彬 ^4,

1.
杭州海关技术中心, 浙江杭州 310016;
2.
浙江省检验检疫科学技术研究院, 浙江杭州 310016;
3.
浙江立德产品技术有限公司, 浙江杭州 310016;
4.
福建农林大学蜂学学院, 福建福州 350002

通讯作者: 侯建波, E-mail:xmuhjb@163.com

基金项目:
国家重点研发计划（2017YFF0211000）；浙江出入境检验检疫局科技计划项目（ZK201710X）.

摘要: 建立了固相萃取净化-液相色谱-串联质谱法（SPE-LC-MS/MS）同时测定蜂蜜中芦丁、杨梅素、桑黄素、槲皮素、柚皮素、橙皮素、木犀草素、染料木素、山柰酚、异鼠李素、芹菜素、松属素、汉黄芩素、白杨素、高良姜素、芫花素和阿魏酸含量的方法。蜂蜜经pH 2的盐酸溶液稀释，C₁₈固相萃取柱净化，液相色谱-串联质谱法检测，外标法定量。以空白蜂蜜基质溶液配制0~200 μg/kg的系列标准溶液，线性相关系数大于0.997，方法定量限为20 μg/kg。在蜂蜜样品中进行加标水平为20、40、100 μg/kg的添加回收试验，回收率为64.5%~113%，相对标准偏差为1.4%~14.5%。该方法取样量少、操作简便、快捷，可用于蜂蜜中黄酮类化合物的测定。

关键词:

English

Simultaneous determination of 16 flavonoids and ferulic acid in honey by solid phase extraction and high performance liquid chromatography-tandem mass spectrometry

1.
Technic Center of Hangzhou Customs, Hangzhou 310016, China;
2.
Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China;
3.
Zhejiang Lead Product Technic Co. Ltd., Hangzhou 310016, China;
4.
College of Bee Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China

Corresponding author: HOU Jianbo, xmuhjb@163.com

Received Date: 29 June 2019
Fund Project:
National Key Research and Development Program of China (No. 2017YFF0211000)

Abstract: Flavonoids are polyphenol compounds that are widely distributed in honey; they play an important role in its antioxidant activity and aid in distinguishing various species of honey. An analytical method based on solid phase extraction and high performance liquid chromatography with tandem mass spectrometry (SPE-HPLC-MS/MS) for the simultaneous determination of rutin, myricetin, morin, quercetin, naringenin, hesperetin, luteolin, genistein, kaempferol, isorhamnetin, apigenin, pinocembrin, wogonin, chrysin, galangin, genkwanin, and ferulic acid in honey was developed and validated. The honey samples were diluted with HCl solution (pH 2) and cleaned up on a C₁₈ column by solid phase extraction; the methanol eluent was filtered through a nylon membrane and analyzed by LC-MS/MS on an ODS-3 column (150 mm×4.6 mm, 3 μm). Quantitative detection was performed by LC-MS/MS in the multiple reaction monitoring (MRM) mode under negative electrospray ionization (ESI^-) conditions. The external standard method was used for quantitation. The method validation data were obtained. The calibration standard curve solutions were prepared by honey matrix-matching; the linear range was 0-200 μg/kg, with correlation coefficients of the calibration standard curves greater than 0.997. The limits of quantification (LOQs) of this method were 20 μg/kg. The recoveries were in the range of 64.5%-113%, and the relative standard deviations were 1.4%-14.5% at three spiked levels (20, 40, and 100 μg/kg). The developed method is convenient, rapid, and effective, and it is suitable for the determination and confirmation of flavonoids in honey samples.

Key words:

solid phase extraction (SPE)
/ high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
/ flavonoids
/ honey

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固相萃取-液相色谱-串联质谱法同时测定蜂蜜中16种黄酮类化合物和阿魏酸

通讯作者: 侯建波, E-mail:xmuhjb@163.com

English

Simultaneous determination of 16 flavonoids and ferulic acid in honey by solid phase extraction and high performance liquid chromatography-tandem mass spectrometry

Corresponding author: HOU Jianbo, xmuhjb@163.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

固相萃取-液相色谱-串联质谱法同时测定蜂蜜中16种黄酮类化合物和阿魏酸

通讯作者: 侯建波, E-mail:xmuhjb@163.com

English

Simultaneous determination of 16 flavonoids and ferulic acid in honey by solid phase extraction and high performance liquid chromatography-tandem mass spectrometry

Corresponding author: HOU Jianbo, xmuhjb@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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