title: Determination of tetracyclines residues in honey by on-line solid-phase extraction high-performance liquid chromatography.
abstract: An automated system using on-line solid-phase extraction (SPE) high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection was developed for the determination of tetracyclines (TCs), such as tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC), metacycline (MC), and doxycycline (DC) in honey. One milliliter diluted honey sample was injected into a conditioned C18 SPE column and the matrix was washed out with water for 3 min. By rotation of the switching valve, TCs were eluted and transferred to the analytical column by the chromatographic mobile phase. Chromatographic conditions were optimized. TCs were separated in less than 8 min with a gradient elution using a mixture of 0.8% formic acid and acetonitrile. The UV detection was performed at 365 nm. The conditions for on-line SPE, including solvent and total time for loading sample and washing matrix were also optimized. Time for extraction and separation decreased greatly. For the five kinds of TCs, the limits of detection (LODs) at a signal-to-noise of 3 ranged from 5 to 12 ng g(-1). The relative standard deviations (R.S.D.) for the determination of TCs ranged from 3.4 to 7.1% within a day and ranged from 3.2 to 8.9% in 3 days, respectively.
authors.affiliation: College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, PR China.
authors.forename: Jiantao
authors.initials: J
authors.lastname: Li
authors.forename: Ligang
authors.initials: L
authors.lastname: Chen
authors.forename: Xiao
authors.initials: X
authors.lastname: Wang
authors.forename: Haiyan
authors.initials: H
authors.lastname: Jin
authors.forename: Lan
authors.initials: L
authors.lastname: Ding
authors.forename: Kun
authors.initials: K
authors.lastname: Zhang
authors.forename: Hanqi
authors.initials: H
authors.lastname: Zhang
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001331:Automation; D002751:Chlortetracycline / Q000032:analysis; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004318:Doxycycline / Q000032:analysis; D005504:Food Analysis / Q000379:methods*; D005561:Formates / Q000737:chemistry; D006722:Honey / Q000032:analysis*; D008690:Methacycline / Q000032:analysis; D010118:Oxytetracycline / Q000032:analysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry; D013754:Tetracyclines / Q000032:analysis*; D013997:Time Factors
chemical_list: D000097:Acetonitriles; D000900:Anti-Bacterial Agents; D005561:Formates; D012997:Solvents; D013754:Tetracyclines; C030544:formic acid; D008690:Methacycline; D004318:Doxycycline; D002751:Chlortetracycline; D010118:Oxytetracycline; C032159:acetonitrile