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

1. [1] Zhao L F, Xu Y Y, Dong R, et al. Food Science, 2013, 34(7):330 赵立夫, 徐云友, 董蕊, 等. 食品科学, 2013, 34(7):330
2. [2] Ye X Z, Wang Q, Yuan Y W. et al. Chinese Journal of Pharmaceutical Analysis, 2010, 30(4):767 叶雪珠, 王强, 袁玉伟, 等. 药物分析杂志, 2010, 30(4):767
3. [3] Yue J P, Gao H, Wang D D, et al. Journal of Food Science and Technology, 2018, 36(3):48 岳锦萍, 高寒, 王丹丹, 等. 食品科学技术学报, 2018, 36(3):48
4. [4] Gong H, Luo D H, Xian Y P, et al. J Agric Food Chem, 2016, 64:3258
5. [5] Fei X Q, Wu B, Shen C Y, et al. Chinese Journal of Chromatography, 2011, 29(1):15 费晓庆, 吴斌, 沈崇钰, 等. 色谱, 2011, 29(1):15
6. [6] Janaína M S, Evandro L S, Gilmardes M, et al. Food Res Int, 2016, 84:61
7. [7] Francine M B, Rui C Z, Bruna W B, et al. LWT-Food Sci Technol, 2016, 65:333
8. [8] Zehra C, Oktay Y, Huseyin S, et al. Food Chem, 2015, 180:133
9. [9] Liang X W, Li Q Q, Gao J L, et al. Food Science, 2018, 39(8):141 梁馨文, 李强强, 高景林, 等. 食品科学, 2018, 39(8):141
10. [10] Guo X L, Luo L P, Leng T T, et al. Natural Product Research and Development, 2010, 22(4):665 郭夏丽, 罗丽萍, 冷婷婷, 等. 天然产物研究与开发, 2010, 22(4):665
11. [11] Isabel E, Melinda K, Marisol J B, et al. Food Res Int, 2011, 44:1504
12. [12] Oroian M, Sorina P. Comput Electron Agr, 2017, 138:148
13. [13] Sun C Z, Wang C, Cai Z Z, et al. Food Science, 2013, 34(10):281 孙崇臻, 王超, 蔡子哲, 等. 食品科学, 2013, 34(10):281
14. [14] Ouchemoukh S, Amessis-Ouchemoukh N, Gomez-Romero M, et al. LWT-Food Sci Technol, 2017, 85:460
15. [15] Wang X X, Zhou Y, Yu T T, et al. Chinese Journal of Pharmaceutical Analysis, 2016, 36(12):2180 王笑笑, 周勇, 俞婷婷, 等. 药物分析杂志, 2016, 36(12):2180
16. [16] Yan L J, Xu D M, Xue X F, et al. Chinese Journal of Chromatography, 2019, 37(6):589 严丽娟, 徐敦明, 薛晓锋, 等. 色谱, 2019, 37(6):589
17. [17] Wang Q, Li Z, Dang X Q, et al. Food Science, 2017, 38(14):164 王琴, 李治, 党晓群, 等. 食品科学, 2017, 38(14):164
18. [18] Wang X X, Yan W H, Huang H, et al. Chinese Journal of Pharmaceutical Analysis, 2017, 37(5):796 王笑笑, 颜伟华, 黄华, 等. 药物分析杂志, 2017, 37(5):796
19. [19] Truchado P, Vit P, Ferreresa F, et al. J Chromatogr A, 2011, 1218:7601
20. [20] Truchado P, Tourn E, Gallez L M, et al. J Agric Food Chem, 2010, 58:12678
21. [21] Stahnke H, Kittlaus S, Kempe G, et al. Anal Chem, 2012, 84(3):1474

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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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