GC/MS combined with chemometrics methods for quality control of Schizonepeta tenuifolia Briq: Determination of essential oils

A simple and rapid gas chromatography/mass spectrometry (GC/MS) analysis method was developed for the determination of essential oils in the crude extract of Schizonepeta tenuifolia Briq (Sch.t.Briq). Five major volatiles (menthone, pulegone, 2-hydroxy-2-isopropenyl-5-methylcylohexanone, cis-pulegone oxide, and schizonal) were extracted and isolated from Sch.t.Briq as marker compounds for use in the quality control of herbal medicines. Various extraction techniques, such as solvent immersion, mechanical shaking, and sonication, were evaluated, 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 1000 μg/mL for menthone and pulegone, and between 2.5 and 75.0 μg/mL for 2-hydroxy-2-isopropenyl-5-methylcylohexanone, cis-pulegone oxide, and schizonal. 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 0.40–0.50 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 2.5 μg/mL at a σ/s of 10. On the basement of method validation, 21 samples of Sch.t.Briq 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 21 different Sch.t.Briq samples in order to classify samples that were collected from different regions.