title: Simultaneous determination of furfural, acetic acid, and 5-hydroxymethylfurfural in corncob hydrolysates using liquid chromatography with ultraviolet detection.
abstract: A single-laboratory validation study was conducted using HPLC for detecting and quantifying acetic acid, furfural, and 5-hydroxymethylfurfural (HMF) in corncob hydrolysates. A pretreatment procedure using dilute sulfuric acid was optimized for corncob hydrolysis. The final hydrolysates were analyzed by HPLC using a C18 RP column with aqueous 0.01% (v/v) H2SO4-CH3OH (95 + 5) as the mobile phase at a flow rate of 1 mL/min. The wavelengths for detecting the three compounds were changed to their optimal UV detection wavelengths at the time of elution. The wavelength detection adjustments were as follow: 205 nm (0 to 4 min); 284 nm (4 to 7 min); and 276 nm (7 to 10 min). Separation was achieved with a chromatographic run time of 10 min. The calibration curves for the three compounds had correlation coefficients (r2) > or = 99.8%. The analytical range, as defined by the calibration curves, was 0.5-10 mg/L for acetic acid, 0.4-22 mg/L for furfural, and 0.1-18 mg/L for HMF. The LODs for acetic acid, furfural, and HMF were estimated to be 0.05, 0.03, and 0.02 mg/L, respectively; the LOQs were 0.196, 0.135, and 0.074 mg/L, respectively. The RSD values for the intraday precision study ranged from 0.31 to 2.22%, and from 0.57 to 2.43% for the interday study. The mean recovery rates in all compounds were between 100.08 and 101.49%.
authors.forename: Bo-Yu
authors.initials: BY
authors.lastname: Dong
authors.forename: Ye-Fu
authors.initials: YF
authors.lastname: Chen
authors.forename: Chang-Chun
authors.initials: CC
authors.lastname: Zhao
authors.forename: Shi-Jie
authors.initials: SJ
authors.lastname: Zhang
authors.forename: Xue-Wu
authors.initials: XW
authors.lastname: Guo
authors.forename: Dong-Guang
authors.initials: DG
authors.lastname: Xiao
mesh_terms: D019342:Acetic Acid / Q000032:analysis*; D018533:Biomass; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D005662:Furaldehyde / Q000031:analogs & derivatives* / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D006868:Hydrolysis; D008031:Lignin / Q000737:chemistry; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet; D013464:Sulfuric Acids; D018505:Waste Management; D003313:Zea mays / Q000737:chemistry
chemical_list: D013464:Sulfuric Acids; C036909:lignocellulose; C008046:5-hydroxymethylfurfural; D008031:Lignin; D005662:Furaldehyde; C033158:sulfuric acid; D019342:Acetic Acid