Enrofloxacin Ofloxacin 1. 4 Sarafloxacin Sparfloxacin Ultimate XB - C mm 2. 1 mm Difloxacin Cinoxacin Nalidixic 5 μm 30 2 mmol /L acid

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1 Sep Chinese Fishery Quality and Standards Vol. 2 No * ESI SRM ~ 200 ng /ml 1. 0 μg /kg 2. 0 μg /kg μg /kg 1. 0 μg /kg % ~ 108% % ~ 13. 1% S912 A Quinolones 200 μg /kg 300 μg /kg 100 μg /kg 500 μg /kg 300 μg /kg 30 μg /kg 4 ELISA 5-6 HPLC 7-12 HPLC /MS /MS AE 21 CE 19 - HPLC /MS / 200 μg /kg MS 100 μg /kg 300 μg μg /kg 30 μg /kg 100 μg /kg 100 μg /kg μg /kg 50 μg /kg 50 ~ 100 μg /kg 20 μg /kg Oxolinic acid Flumequine Norfloxacin Enoxacin μg /kg Ciprofloxacin Pefloxacin Lomefloxacin Danofloxacin qianzhuozhen@ 126. com E - mail wcy@ fjscs. ac. cn

2 Enrofloxacin Ofloxacin 1. 4 Sarafloxacin Sparfloxacin Ultimate XB - C mm 2. 1 mm Difloxacin Cinoxacin Nalidixic 5 μm 30 2 mmol /L acid Orbifloxacin Marbofloxacin Fleroxacin Pipemidic acid Dr > 92% Milli - Q 99 ml 1 ml 2 mmol /L % Accela TSQ Quantum Access /min /% Thermo Fisher Time Mettler Toledo mg 200 μl 100 ml 100 μg /ml ± g 100 ml 10 g 20 ml r /min 1 min 8 min r /min 5 min 20 ml 1 30 ml 2 mmol /L 0. 2% - 2 min 100 ml ml % ml /min 10 μl 1 ml r /min 0. μm - 28 min 1 Tab. 1 HPLC HPLC mobile phase gradients /% Acetonitrile 2 mmol /L Ammonium acetate % MS IKA PL AB204 - E Formic acid in water V Pa μl 10 4 Pa ml 1 μg /ml 10 V SRM Q Da Q Da Pa 2

3 Tab. 2 2 The optimization parameters of SRM of the analytes m /z Parent ion m /z Product ions * * * 303* * * 265* * * * 299* * * 217* * * 72* * * 189 * / ev Collision energy μg /ml 19 M + H + LC /MS / MS V /V 99 1 V /V 4 1 ml 99 1 V /V ng / ml x y 3 3 S /N 0. 5 μg /kg 1. 0 μg /kg 10 S /N 1. 0 μg /kg 2. 0 μg /kg

5 Tab. 3 Linear regression equation Regression analysis and correlation coefficient /R 2 Correlation coefficient Linear regression equation /R 2 Correlation coefficient y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x Oreochromis spp Scylla serata Penaeus van- namei Anguilla japonicus Haliotis discus 6 Trionyx sinensis Crassostrea gigas d 5μg /kg 6 4 Tab. 4 n = 6 Recoveries and intraday precisions of spiked tissue / / /% /% /% /% μg kg - 1 μg kg - 1 Mean recovery rate RSD Mean recovery rate RSD Spiked Spiked 1 LOQ LOQ LOQ LOQ LOQ LOQ LOQ LOQ LOQ LOQ

6 Tab. 4 Continued / / /% /% /% /% μg kg - 1 μg kg - 1 Mean recovery rate RSD Mean recovery rate RSD Spiked Spiked 1 LOQ LOQ LOQ LOQ LOQ LOQ LOQ LOQ LOQ LOQ Tab. 5 5 n = 6 Recoveries and interday precisions of spiked tissue 6 /% /% Recovery rate Mean recovery rate /% /78. 4 /80. 1 /72. 1 /79. 5 / /80. 4 /82. 9 /81. 7 /85. 0 / /89. 2 /90. 5 /83. 3 /103 / /90. 6 /85. 6 /79. 9 /93. 0 / /94. 5 /89. 2 /81. 2 /79. 9 / /91. 4 /92. 6 /81. 9 /82. 7 / /98. 7 /89. 8 /80. 4 /82. 1 / /90. 1 /92. 5 /89. 7 /78. 5 / /98. 0 /87. 2 /88. 4 /79. 1 / /101 /87. 5 /90. 1 /93. 5 / /89. 1 /90. 5 /89. 2 /92. 4 / /90. 5 /98. 2 /86. 5 /80. 7 / /90. 5 /84. 1 /83. 9 /76. 1 / /90. 1 /84. 4 /90. 6 /92. 7 / /105 /79. 4 /80. 4 /90. 7 / /93. 8 /96. 5 /75. 1 /82. 0 / /86. 4 /82. 1 /90. 7 /91. 5 / /89. 5 /97. 2 /90. 9 /98. 2 / /80. 4 /90. 6 /92. 4 /88. 0 / RSD

8 Zeng Z L Dong A G Yang G X et al. Simultaneous determination of nine fluoroquinolones in egg white and egg yolk by liquid chromatography with fluorescence detection 19 J. J Chromatogr B Pecorelli I Galarini R Bibi R et al. Simultaneous determination of 13 quinolones from feeds using accelerated 2006 solvent extraction and liquid chromatography J. Anal 16 Chim Acta / J J J Clemente M Hermo M P Barrón D et al. Confirmatory 1. and quantitative analysis using experimental design for the J extraction and liquid chromatography - UV liquid chromatography - mass spectrometry and liquid chromatogra- 2 WTO /TBT - SPS. EB/OL http / /www. phy - mass spectrometry / mass spectrometry determination tbt - sps. gov. cn/jpmrl /MRLS/Pages/MRLSsearch. aspx. of quinolones in turkey muscle J. J Chromatogr A S Samanidou V Evaggelopoulou E Trotzmuller M et al. 4. M. Multi - residue determination of seven quinolones antibiotics in gilthead seabream using liquid chromatography ELIASA tandem mass spectrometry J. J Chromatogr A 2008 J Johnston L Mackay L Croft M. Determination of quinolones and fluoroquinolones in fish tissue and seafood by 6. J high - performance liquid chromatography with electros J Chromatogr A Toussaint B Bordin G Janosi A et al. Validation of a J liquid chromatography - tandem mass spectrometry method for the simultaneous quantification of 11 fluoro quinolo- 8. ne antibiotics in swine kidney J. J Chromatogr A J J Yorke J C Froc P. Quantitation of nine quinolones in chicken tissues by high - performance liquid chromatography with fluorescence detection J. J Chromatogr A pray ionisation tandem mass spectrometric detection J / J Beltagi A M. Determination of the antibiotic drug pefloxacin in bulk form tablets and human serum using square wave cathodic adsorptive stripping voltammetry J. J

9 Pharm Biomed Anal Barbosa J Barrón D et al. Determination of difloxacin and sarafloxacin in chicken muscle using solid - phase extraction and capillary electrophoresis J. J Chromatogr B Determination of nineteen quinolones in fishery products by high performance liquid chromatography - tandem mass spectrometry QIAN Zhuozhen 1 3 ZHU Shichao 2 WEI Bojuan 2 TANG Shuifen 1 LUO Fangfang 2 WU Chengye 1* 1. Fisheries Research Institute of Fujian Xiamen China 2. College of Engineering Technology Jimei University Xiamen China 3. College of Materials Xiamen University Xiamen China Abstract A method has been developed for detecting nineteen quinolones including oxolinic acid flumequine norfloxacin enoxacin ciprofloxacin pefloxacin lomefloxacin danofloxacin enrofloxacin ofloxacin sarafloxacin sparfloxacin difloxacin cinoxacin orbifloxacin marbofloxacin nalidixic acid fleroxacin and pipemidic acid by high performance liquid chromatography - tandem mass spectrometry. Samples were extracted with acidified acetonitrile cleaned up with hexane. Analyte identification and quantification were performed using selected reaction monitoring SRM with one precursor ion and two product ions as identifiers and electrospray ionization in positive mode. There are good linear correlations between the peak areas and concentrations of quinolones the calibration coefficients are above the dynamic linear range is ng /ml. The limits of detection are 0. 5 μg /kg for quinolones and the limits of quantification is 1. 0 μg / kg. The average recoveries ranged from 76. 3% to 108% and their relative standard deviations were between % and 13. 1%. The method can be used to identify and quantify the metabolites of quinolones in aquatic products with satisfactory sensitivity accuracy and precision. Chinese Fishery Quality and Standards Key words high performance liquid chromatography - tandem mass spectrometry quinolones fishery products residues Corresponding author WU Chengye. E - mail wcy@ fiscs. ac. cn

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0.

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0. 118 217 5 38 1 DOI 1.3969/j.issn.5-6521.217.1.28 Food Research And Development 1 2 1 2 1 2 1 2 1 2 1 2 1. 731 2. 731 - UPLC-MS/MS 5. 1 mol/l ProElut PXC 5 % - Thermo Hypersil Gold mm 2.1 mm 1.9 μm ESI