title: [Simultaneous determination of chloramphenicol, thiamphenicol, and florfenicol residues in animal tissues by gas chromatography/mass spectrometry].
abstract: A method was developed for the simultaneous determination of chloramphenicol (CAP), thiamphenicol (TAP), and florfenicol (FF) residues in animal tissues using gas chromatography/mass spectrometry (GC/MS) with chemical ionization source in negative mode. The homogenized samples were extracted with ethyl acetate and the extracts were partitioned with n-hexane to remove lipids. Further cleanup was performed on a florisil cartridge and the purified samples were derivatized with Sylon BFT [N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA)-trimethylchlorosilane (TMCS), 99: 1, v/v] in toluene. Meta-nitrochloramphenicol (m-CAP) was used as the internal standard for the determination. Selected ion monitoring (SIM) was used for detection, ions were chosen, respectively, for the monitoring at m/z 432, 466, 468, 470 for m-CAP, m/z 376, 378, 466, 468 for CAP, m/z 409, 411, 499, 501 for TAP, and m/z 339, 341, 429, 431 for FF. Quantitative ions were selected at m/z 466 for CAP and m-CAP, at m/z 339 for FF and at m/z 409 for TAP. The detection limits were 0.03 microg/kg for CAP, 0.2 microg/kg for FF and TAP. The correlation coefficients were above 0.99 for the calibration curves of the medicines. The linear ranges were 0.1 - 8.0 microg/kg for CAP and 0.2 - 4.0 microg/kg for FF and TAP. The reproducibilities of the compounds within a batch were 5.5%, 10.4%, and 8.8% for CAP, FF, and TAP respectively, while the corresponding values between the batches were 7.4%, 20.7%, and 19.1%. The recoveries were 80.0% - 111.5%, and the relative standard deviations were 1.2% - 15.4%. The method is applicable for detection of the residues in animal derived food, such as pork, poultry and aquatic products.
authors.affiliation: Chinese Academy of Inspection and Quarantine, Beijing 100025, China. shiner_lp@163.com
authors.forename: Peng
authors.initials: P
authors.lastname: Li
authors.forename: Yueming
authors.initials: Y
authors.lastname: Qiu
authors.forename: Huixia
authors.initials: H
authors.lastname: Cai
authors.forename: Ying
authors.initials: Y
authors.lastname: Kong
authors.forename: Yingzhang
authors.initials: Y
authors.lastname: Tang
authors.forename: Daning
authors.initials: D
authors.lastname: Wang
authors.forename: Mengxia
authors.initials: M
authors.lastname: Xie
mesh_terms: D000818:Animals; D002701:Chloramphenicol / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006586:Hexanes; D057230:Limit of Detection; D013552:Swine; D013839:Thiamphenicol / Q000031:analogs & derivatives* / Q000032:analysis*
chemical_list: D006586:Hexanes; C026385:n-hexane; D002701:Chloramphenicol; C035534:florfenicol; D013839:Thiamphenicol