title: Determination of ultra-trace organic acids in Masson pine (Pinus massoniana L.) by accelerated solvent extraction and liquid chromatography-tandem mass spectrometry.
abstract: An accelerated solvent extraction (ASE)-solid-phase extraction (SPE)-liquid chromatography with electrospray ionization-tandem mass spectrometry (ASE-SPE-LC-ESI-MS/MS) methodology was developed for the extraction, cleanup and quantification of ultra-trace organic acids in Masson pine (Pinus massoniana L.) tissues. The separation was carried out on a Bio-Rad Aminex HPX-87H sulfonic column with an eluent containing 5 mmol L(-1) H₂SO₄ at a flow rate of 0.5 mL min(-1). A linear ion trap mass spectrometer equipped with electrospray ionization (ESI) source was operated in negative ion mode, and the six organic acids were eluted within 20 min. ASE extraction, SPE cleanup and LC-ESI-MS/MS analysis conditions were optimized to obtain reliable information about plant organic acid composition. Selective reaction monitoring (SRM) was employed for quantitative measurement. Intra-day precisions averaged 6.7%, and inter-day precisions were 2.1-10.7% for organic acid measurements in the pine samples. External standard calibration curves were linear over the range of 16.5-5000 ng L(-1), and detection limits based on a signal-to-noise ratio of three were at 0.5-5.0 ng L(-1). The results obtained showed the sensibility of the method was better than that of previously described HPLC methodology, and had no significant matrix effect. The proposed ASE-SPE-LC-ESI-MS/MS method is sensitive and reliable for the determination of ultra-trace organic acids in plant samples, despite the presence of the particularly complex matrix.
authors.affiliation: College of Biology and Environment, Nanjing Forestry University, Nanjing 210037, People's Republic of China.
authors.forename: Shuiliang
authors.initials: S
authors.lastname: Wang
authors.affiliation: Gas Technology Institute, 1700 S. Mt. Prospect Road, Des Plaines, IL 60018, USA.
authors.forename: China Q
authors.initials: CQ
authors.lastname: Fan
authors.affiliation: College of Biology and Environment, Nanjing Forestry University, Nanjing 210037, People's Republic of China. Electronic address: wp_lh@aliyun.com.
authors.forename: Ping
authors.initials: P
authors.lastname: Wang
mesh_terms: D002264:Carboxylic Acids / Q000032:analysis* / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods*; D057230:Limit of Detection; D016014:Linear Models; D028223:Pinus / Q000737:chemistry*; D015203:Reproducibility of Results; D059629:Signal-To-Noise Ratio; D052616:Solid Phase Extraction; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D002264:Carboxylic Acids; D012997:Solvents
keywords: Accelerated solvent extraction; Liquid chromatography–tandem mass spectrometry; Masson pine (Pinus massoniana L.); Organic acids