title: Simultaneous quantification of polymethoxylated flavones and coumarins in Fructus aurantii and Fructus aurantii immaturus using HPLC-ESI-MS/MS.
abstract: The major lipid-soluble constituents in Fructus aurantii (zhiqiao) and Fructus aurantii immaturus (zhishi) are polymethoxylated flavones (PMFs) and coumarins. In the present study, a high-performance liquid chromatography with electrospray ionization tandem mass spectrometry method was developed to quantify PMFs (nobiletin, tangeretin, 5-hydroxy-6,7,8,4'-tetramethoxyflavone, and natsudaidai) and coumarins (marmin, meranzin hydrate, and auraptene) simultaneously. PMFs and coumarins were detected by electrospray ionization tandem mass spectrometry in positive ion mode and quantified with multiple reaction monitor. Samples were separated on a Diamonsil C₁₈ (150 mm × 4.6 mm, 5 μm) column using acetonitrile and formic acid-water solution as a mobile phase in gradient mode with a flow rate at 0.5 mL/min. All calibration curves showed good linearity (r² > 0.9977) within the test ranges. Variations of the intraday and interday precisions were less than 4.07%. The recoveries of the components were within the range of 95.79%-105.04% and the relative standard deviations were less than 3.82%. The method developed was validated with acceptable accuracy, precision, and extraction recoveries and can be applied for the identification and quantification of four PMFs and three coumarins in citrus herbs.
authors.affiliation: The Key Laboratory of Modern Preparation of TCM of Ministry of Education, Jiangxi University of Traditional Chinese Medicine, Nanchang, Jiangxi Province 330004, China.
authors.forename: Hai-Fang
authors.initials: HF
authors.lastname: Chen
authors.forename: Wu-Gang
authors.initials: WG
authors.lastname: Zhang
authors.forename: Jin-Bin
authors.initials: JB
authors.lastname: Yuan
authors.forename: Yan-Gang
authors.initials: YG
authors.lastname: Li
authors.forename: Shi-Lin
authors.initials: SL
authors.lastname: Yang
authors.forename: Wu-Liang
authors.initials: WL
authors.lastname: Yang
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D002957:Citrus / Q000737:chemistry*; D003374:Coumarins / Q000737:chemistry / Q000302:isolation & purification*; D004365:Drugs, Chinese Herbal / Q000737:chemistry / Q000302:isolation & purification*; D047309:Flavones / Q000737:chemistry / Q000302:isolation & purification*; D005638:Fruit / Q000737:chemistry; D057230:Limit of Detection; D015394:Molecular Structure; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000295:instrumentation / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*
chemical_list: D003374:Coumarins; D004365:Drugs, Chinese Herbal; D047309:Flavones