Development of Fingerprints for Quality Control of Acorus species by Gas Chromatography/Mass Spectrometry

Abstract

An effective analytical method of gas chromatography/mass spectrometry (GC/MS) was developed for the rapid determination of essential oils in the crude extract of Acorus species (Acorus gramineus, Acorus tatarinowii, and Acorus calamus). Major phenypropanoids (β,α-asarone isomers, euasarone, and methyleugenol) and β-caryophyllene in Acorus species were used as marker compounds and determined for the quality control of herbal medicines. To extract marker compounds, various extraction techniques such as solvent immersion, mechanical shaking, and sonication were compared, and the greatest efficiency was observed with sonication extraction using petroleum ether. The dynamic range of the GC/MS method depended on the specific analyte; acceptable quantification was obtained between 10 and 2000 μg/mL for β-asarone, 10 and 500 μg/mL for α-asarone, 10 and 200 μg/mL for methyleugenol, and between 5 and 100 μg/mL for β-caryophyllene. The method was deemed satisfactory by inter-and intra-day validation and exhibited both high accuracy and precision, with a relative standard deviation < 10%. Overall limits of detection were approximately 0.34-0.83 μg/mL, with a standard deviation (σ)-to-calibration slope (s) ratio (σ/s) of 3. The limit of quantitation in our experiments was approximately 1.13-3.20 μg/mL at a σ/s of 10. On the basement of method validation, 20 samples of Acorus species collected from markets in Korea were monitored for the quality control. In addition, principal component analysis (PCA) and hierarchical cluster analysis (HCA) were performed on the analytical data of 20 different Acorus species samples in order to classify samples that were collected from different regions.

Cytotoxic Lignans and Sesquiterpenoids from the Rhizomes of Acorus tatarinowii

“…S2-S15, Supporting Information). The major components were α-asarone and β-asarone, as expected from our work on this species collected from Anhui province [19] and the results of others [3,[20][21][22][23]. Minor compounds 2-4 (see below) and tatanna A [5] were also identified from the EtOH extract based on mass spectra (Figs.…”

Qualitative and quantitative analysis of the major constituents in Acorus tatarinowii Schott by HPLC/ESI‐QTOF‐MS/MS

“…Owing to its biological activities and popular use, it is important to peform quantitative and qualitative studies of the constituents of ATS. Many studies have mainly focused on the analysis of sesquiterpenoids and phenylpropanoids from ATS (Lao et al ., ; Venskutonis and Dagilyte, ; Yu et al ., ; Lee et al ., and ; Deng et al ., ). Since high‐performance liquid chromatography–mass spectrometry (HPLC‐MS) has become a powerful tool for qualitative analysis of TCM and metabolites owing to its high resolution, accuracy and reproducibility (Ling et al ., ; Fu et al ., ; Chen et al ., ; Bagnall et al ., ; Martinez Bueno et al ., ; Qi et al ., ), we have developed a method using a high‐performance liquid chromatography coupled with electrospray ionization quadrupole time‐of‐flight mass spectrometry (HPLC/ESI‐QTOF‐MS/MS) technique for a comprehensive qualitative analysis of ATS.…”

Separation ofcis- andtrans-Asarone fromAcorus tatarinowiiby Preparative Gas Chromatography

“…And the mass spectra of furanodienone and curzerenone were very similar, which induced the wrong identification of furanodienone as curzerenone without reference compound [ 24 ]. To date, HPLC [ 25 – 28 ] and GC-MS [ 29 – 32 ] are two most frequently used techniques for the analysis of asarone. Furthermore, asarone isomers also show similar mass spectra [ 33 ], which make the identification of those compounds difficult when the reference compounds were absence.…”