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DOI10.1016/j.jchromb.2019.01.018
Determination of total florfenicol residues as florfenicol amine in bovine tissues and eel by liquid chromatography-tandem mass spectrometry using external calibration
Saito-Shida, Shizuka; Shiono, Kouji; Narushima, Jumpei; Nemoto, Satoru; Akiyama, Hiroshi
通讯作者Saito-Shida, Shizuka
来源期刊JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
ISSN1570-0232
EISSN1873-376X
出版年2019
卷号1109页码:37-44
英文摘要A reliable liquid chromatography-tandem mass spectrometry method was developed to determine total florfenicol residues in bovine tissues and eel. Florfenicol and its metabolites (florfenicol amine, monochloroflorfenicol, florfenicol oxamic acid, and florfenicol alcohol) were analyzed as the marker residue, florfenicol amine, as defined by several regulatory agencies. After hydrolysis with hydrochloric acid, samples were defatted and subjected to solid-supported liquid extraction and Oasis MCX-cartridge cleanup before analysis. The method was validated for florfenicol and its metabolites at two levels in eel and bovine muscle, fat, and liver. Excellent recoveries were obtained (93-104%), with relative standard deviations of < 6% for all compounds. Negligible matrix effects and minimal analyte loss during sample preparation enabled accurate quantification by external calibration using solvent standards. No interfering peaks were observed around the retention time of florfenicol amine, indicating the high selectivity of the method. Retention times in the spiked samples corresponding to that of the calibration standard in solvent did not exceed +/- 0.1 min. Ion ratios from the spiked sample were within +/- 10% (relative) of the calibration standards. Calibration curves were linear in the range of 0.5 to 100 ng/mL, with coefficients of determination higher than 0.998. The limits of quantification and limits of detection of the proposed method were estimated to be 0.01 mg/kg and 0.0005 mg/kg, respectively, in all food samples. Thus, the developed method is considered reliable and suitable for regulatory use.
英文关键词Florfenicol Florfenicol amine Hydrolysis LC-MS/MS
类型Article
语种英语
国家Japan
收录类别SCI-E
WOS记录号WOS:000461411800005
WOS关键词SWINE MUSCLE ; GAS-CHROMATOGRAPHY ; IN-VITRO ; THIAMPHENICOL ; CHLORAMPHENICOL ; FISH ; EXTRACTION ; VALIDATION ; POULTRY ; SHRIMP
WOS类目Biochemical Research Methods ; Chemistry, Analytical
WOS研究方向Biochemistry & Molecular Biology ; Chemistry
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/216840
作者单位Natl Inst Hlth Sci, Div Foods, Kawasaki Ku, Tonomachi 3-25-26, Kawasaki, Kanagawa 2109501, Japan
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GB/T 7714
Saito-Shida, Shizuka,Shiono, Kouji,Narushima, Jumpei,et al. Determination of total florfenicol residues as florfenicol amine in bovine tissues and eel by liquid chromatography-tandem mass spectrometry using external calibration[J],2019,1109:37-44.
APA Saito-Shida, Shizuka,Shiono, Kouji,Narushima, Jumpei,Nemoto, Satoru,&Akiyama, Hiroshi.(2019).Determination of total florfenicol residues as florfenicol amine in bovine tissues and eel by liquid chromatography-tandem mass spectrometry using external calibration.JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES,1109,37-44.
MLA Saito-Shida, Shizuka,et al."Determination of total florfenicol residues as florfenicol amine in bovine tissues and eel by liquid chromatography-tandem mass spectrometry using external calibration".JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES 1109(2019):37-44.
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