Separation and quantitation of notopterol enantiomers in notopterygii rhizoma et radix using solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry

• Published in: Journal of pharmaceutical and biomedical analysis 2020-07, Vol.186, p.113255-113255, Article 113255
• Main Authors: Cai, Liangzhao, Lun, Jia, Liu, Yanru, Guo, Xingjie
• Format: Article
• Language: English
• Subjects: Artemisia - chemistry; Chromatography, High Pressure Liquid; Coumarins - chemistry; Drugs, Chinese Herbal; Enantioseparation; LC–MS/MS; Limit of Detection; Medicine, Chinese Traditional; Notopterol; Notopterygii; Quantitative analysis; Reference Standards; Reproducibility of Results; Rhizoma et radix; Rhizome - chemistry; Solid Phase Extraction; Stereoisomerism; Tandem Mass Spectrometry
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2020.113255

•Enantiomeric separation of notopterol in Notopterygii Rhizoma et Radix (NRR) was studied firstly by using Chiralpak IA column.•It was the first time that the contents of notopterol enantiomers in NRR samples from different regions were determined by using LC–MS/MS method.•A thin-layer chromatography method was firstly developed to prepare the (+)-notopterol, then the configuration confirmation was determined by circular dichroism spectrum to confirm the elution order.•Statistical method (T-test) was used for significance testing of (+)/(-) value in NRR samples from different regions, and the ratios of (+)/(-) were demonstrated remarkable differences. In this study, a specific, sensitive, and reliable high performance liquid chromatography-tandem mass spectrometry method has been developed and validated for the quantitative determination of notopterol enantiomers in Notopterygii Rhizoma et Radix. Solid-phase extraction was used for the extraction of notopterol enantiomers from Notopterygii Rhizoma et Radix. Enantiomeric separation of notopterol was achieved on a Chiralpak IA column with the mobile phase consisting of acetonitrile-water (50:50, v/v) at a flow rate of 0.6 mL/min. Quantification was performed on a triple quadrupole tandem mass spectrometry equipped with an electrospray ionization source in the positive ionization and multiple reaction monitoring mode. The lower limit of quantification and lower limit of detection were 0.09 and 0.04 mg/g for each enantiomer in NRR samples. And each enantiomer showed good linearity (R2≥0.999) in the range of 0.09–9.55 mg/g. The precision, repeatability, and stability were all within satisfaction. The average recoveries of (-)-notopterol and (+)-notopterol were demonstrated to be 99.3 % and 101.1 %, respectively, with the relative standard deviations less than 5.0 %. Finally, the validated method was successfully applied to the quantification of notopterol enantiomers in Notopterygii Rhizoma et Radix from different sources.