Identification of Compounds in Commercial Kava Extracts by Gas Chromatography with Electron Ionization High-Resolution Mass Spectrometry

Abstract

This paper discusses the identification of kava lactones and related compounds by gas chromatography (GC) and quadrupole time-of-flight mass spectrometry (QTOFMS) with an electron ionization source. Three herbal preparations from different sources were analyzed by both GC-low-resolution MS and GC-high-resolution MS. The exact mass measurements generated with a research QTOFMS with mass accuracies in the low ppm range were combined with the isotope abundance ratios to confirm the presence of kava lactones and to identify additional compounds present in the Kava extracts. Although the availability of standards is of upmost importance to unequivocally confirm compound identities, the combination of accurate mass (< 3 ppm average mass accuracy), isotope abundance ratios, high resolution (>10,000) and literature information on the approximate composition of the herbal extracts provides a powerful analytical tool to help identify organic compounds in herbal extracts.

Rapid detection and validated quantification of psychoactive compounds in complex plant matrices by direct analysis in real time‐high resolution mass spectrometry – Application to “Kava” psychoactive pepper products

“…Although a variety of techniques have been applied to qualitative and quantitative studies of kavalactones in Kava products, thermal decomposition, low sensitivity and limitations regarding separation time and peak resolution have proven troublesome in Kava analysis . Near‐infrared reflectance spectroscopy (NIRS) and FTIR with attenuated total reflectance (ATR) have demonstrated advantages including non‐destructiveness, high speed and sensitivity, and involve minimal to no sample preparation for analysis and quantification of major kavalactones .…”

“…Based on spectra (Figure 3) and the corresponding mass measurement data (Table S2, Although a variety of techniques have been applied to qualitative and quantitative studies of kavalactones in Kava products, thermal decomposition, low sensitivity and limitations regarding separation time and peak resolution have proven troublesome in Kava analysis. [18][19][20] Near-infrared reflectance spectroscopy (NIRS) and FTIR with attenuated total reflectance (ATR) have demonstrated advantages including non-destructiveness, high speed and sensitivity, and involve minimal to no sample preparation for analysis and quantification of major kavalactones. 20,29,30 However, the poor stability of yangonin in certain solvent systems and calibration curves with low R 2 values for several major kavalactones remain problematic with these methods.…”

“…The success of these efforts has hinged on the availability of reliable approaches for the identification of Kava products and quantification of individual components. Techniques used have included gas chromatography (GC), [18][19][20] liquid chromatography/mass spectrometry (LC/MS), 21,22 high-performance 10,18,23,24 and ultraperformance 25 liquid chromatography (HPLC and UPLC) and supercritical fluid chromatography (SFC), 18,26 among others. 18,22,[27][28][29][30][31] The approaches differ in terms of speed, sensitivity, selectivity and the extent to which they can be readily applied to both qualitative and quantitative studies, as well as the level of sample pretreatment required.…”

<span>THẨM ĐỊNH PHƯƠNG PH&Aacute;P ĐỊNH LƯỢNG 5,6-DEHYDROKAVAIN TRONG L&Aacute; C&Acirc;Y RIỀNG ẤM (<em>ALPINIA ZEZUMBET</em>) V&Agrave; BỘT RIỀNG ẤM BẰNG KỸ THUẬT SẮC K&Yacute; LỎNG HIỆU NĂNG CAO</span>

“…Trên thế giới, hầu hết các nghiên cứu đã công bố sử dụng kỹ thuật sắc ký lỏng (HPLC) với detector UV-VIS [14], một số ít nghiên cứu sử dụng kỹ thuật sắc ký khí GC/MS [5,6]…”