Analysis of an Adulterated Herbal Medicinal Product Using Ultra-Performance Liquid Chromatography Coupled with QTOF Mass Spectrometry

Abstract

The reports of severe adverse effects and fatalities associated with herbal medicinal products adulterated with synthetic compounds have raised global concerns. The objective of this study is to analyze one commercial herbal medicinal product suspected to be adulterated with synthetic drugs in order to identify potential adulterants, to verify if the product contained the herbs listed as ingredients in label claim and to determine quality consistency among different batches of the product. Analyses of suspected product obtained from seven different batches were performed using ultra performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) with multiple data processing tools and multivariate analyses. In addition, 23 individual powdered herbs (12 as per label claim and 11 suspected herbs), 11 marker compounds of the labeled herbs and five suspected synthetic drugs as adulterants were also concurrently analyzed to have clear understanding of product composition. Based on our analysis, the major ingredients of studied product were found to be 5 synthetic compounds: caffeine, chlorphenamine, piroxicam, betamethasone and oxethazaine. Three of them have been found to exceed their recommended doses. From the herbal composition analysis, GanCao (Glycyrrhizae radix et rhizoma) was found to be the main ingredient, which is not among the claimed 12 herbs that were supposed to be in the product. Other herbs detected as minor ingredients were MuGua (Chaenomelis fructus), DangGui (Angelicae sinensis radix), and HuangQi (Astragali radix), which are among the 12 herbs that were supposed to be in the product. Based on our results we demonstrated that UPLC-QTOF MS is an effective and versatile tool for the analysis of herbal medicinal products. It is highly desirable to have a streamlined process with automatic workflow and fit-for-purpose database to increase efficiency and productivity of sample analysis. Results of this work also highlight the need for the better quality control and regulatory measures to protect consumers from the potentially harmful effects of such adulterated products.

Keywords

• Synthetic adulterants
• Adulteration
• UPLC-QTOF-MS
• Herbal products
• Data independent acquisition
• Multi-Variate Statistical Analysis