Optimization of a solid phase extraction and hydrophilic interaction liquid chromatography-tandem mass spectrometry method for the determination of metformin in dietary supplements and herbal medicines

Ximei Wu; Binghui Zhu; Lin Lu; Weixiong Huang; Daiwen Pang

doi:10.1016/j.foodchem.2012.01.005

Optimization of a solid phase extraction and hydrophilic interaction liquid chromatography-tandem mass spectrometry method for the determination of metformin in dietary supplements and herbal medicines

Food Chem. 2012 Jul 15;133(2):482-8. doi: 10.1016/j.foodchem.2012.01.005. Epub 2012 Jan 18.

Authors

Ximei Wu¹, Binghui Zhu², Lin Lu², Weixiong Huang², Daiwen Pang³

Affiliations

¹ Center for Disease Prevention and Control of Guangdong Province, Guangzhou 510300, China; College of Chemistry and Molecular Sciences, Wuhan University, Luojiashan, Wuhan 430072, China. Electronic address: wxmdwb927@126.com.
² Center for Disease Prevention and Control of Guangdong Province, Guangzhou 510300, China.
³ College of Chemistry and Molecular Sciences, Wuhan University, Luojiashan, Wuhan 430072, China. Electronic address: dwpang@whu.edu.cn.

PMID: 25683423
DOI: 10.1016/j.foodchem.2012.01.005

Abstract

Metformin is one of the most common adulterants found in anti-diabetic dietary supplements and herbal medicines. An analytical method based on hydrophilic interaction chromatography (HILIC)/tandem mass spectrometry was developed and validated for the determination of metformin in dietary supplements and herbal medicines. Sample preparation involved solid phase extraction of the analyte using Plexa PCX cartridges, and cleanup by a primary-secondary amine (PSA) adsorbent for minimization of the matrix effect. Chromatographic separation was performed on a HILIC column using a mixture of 0.025 mol/L ammonium formate (pH 3) and acetonitrile (18:82, v/v) as the mobile phase at flow rate of 0.25 mL/min. The method was validated in four matrices (capsules, honeyed pills, tablets and oral solutions). The method had a good linear range (5-500 ng/mL), and the overall precision and accuracy ranged from 2.2% to 9.9% and 4.6% to 11.3%, respectively.

Keywords: Dietary supplements; HILIC/MS/MS; Herbal medicines; Metformin; Primary–secondary amine adsorbent; Solid phase extraction.

Publication types

Research Support, Non-U.S. Gov't

MeSH terms

Chromatography, Liquid / methods*
Dietary Supplements / analysis*
Herbal Medicine / methods*
Hydrophobic and Hydrophilic Interactions
Metformin / analysis*
Metformin / chemistry
Solid Phase Extraction / methods*
Tandem Mass Spectrometry / methods*

Substances

Metformin