title: Quantitative HPLC method for determining two of the major active phthalides from Ligusticum porteri roots.
abstract: Z-Ligustilide (1) and Z-6,6',7,3'-alpha-diligustilide (2), two of the major active phthalides of the medicinal plant Ligusticum porteri (osha), were chosen for the development and validation of an HPLC-diode array detection method suitable for QC of the crude drug. The method used gradient elution to achieve separation on a Hibar RT LiChrospher 100 C18 column. The LOD values were 29 and 45 microg/mL, and the LOQs were 89 and 125 microg/mL, respectively. The method showed good intraday precision (%RSD: 0.7 for 1 and 3.1 for 2) and interday precision (%RSD: 1.2 for 1 and 1.8 for 2). The method was used for the analysis of 1 and 2 in crude drug samples and several herbal preparations from Mexico and the United States. Quantitative analysis showed that the content of the two phthalides varied significantly among the samples. All the samples contained higher concentrations of 1 (0.15-2.5%) than 2 (0.002-1.0%). The profiles of volatile compounds in the essential oil obtained by hydrodistillation and solid-phase microextraction of L. porteri roots were analyzed by GC-MS. Thirty one chemical constituents (> 99.7% of the total content) were identified in the essential oil, which was characterized by the presence of a high percentage of phthalides (44.61%) and sesquiterpenes (10.69%). The major light volatile components extracted by solid-phase microextraction were monoterpenes.
authors.affiliation: Universidad Nacional Autónoma de México, Facultad de Química, México DF 04510, México.
authors.forename: Isabel
authors.initials: I
authors.lastname: Rivero
authors.forename: Krutzkaya
authors.initials: K
authors.lastname: Juárez
authors.forename: Magda
authors.initials: M
authors.lastname: Zuluaga
authors.forename: Robert
authors.initials: R
authors.lastname: Bye
authors.forename: Rachel
authors.initials: R
authors.lastname: Mata
mesh_terms: D015107:4-Butyrolactone / Q000031:analogs & derivatives* / Q000032:analysis; D001572:Benzofurans; D002851:Chromatography, High Pressure Liquid; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D007202:Indicators and Reagents; D030004:Ligusticum / Q000737:chemistry*; D057230:Limit of Detection; D008800:Mexico; D010936:Plant Extracts / Q000032:analysis; D028321:Plant Preparations / Q000032:analysis; D018517:Plant Roots / Q000737:chemistry; D012015:Reference Standards; D012044:Regression Analysis; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods; D012997:Solvents; D014481:United States
chemical_list: D001572:Benzofurans; D007202:Indicators and Reagents; D010936:Plant Extracts; D028321:Plant Preparations; D012997:Solvents; C523615:levistolide A; C027820:ligustilide; D015107:4-Butyrolactone