建立了加速溶剂萃取-高效液相色谱-串联质谱同时检测鱼肌肉中19种抗生素及2种磺胺代谢产物残留量的分析方法。样品以甲醇为萃取溶剂，采用加速溶剂萃取仪萃取，并在萃取池内以 C18填料作为吸附剂进行同步净化。提取液经冷冻离心去除生物杂质后，经氮吹浓缩、定容，以高效液相色谱-串联质谱分析。采用 Xterra MS C18色谱柱分离，以0.1％（体积分数）甲酸水溶液（含0.1％甲酸铵）为流动相 A，以甲醇-乙腈（1：1，v／v）为流动相 B。方法的加标回收率为55.2％~113.3％，相对标准偏差为0.1％~17.6％（ n=6），方法的检出限为0.003~0.6 ng／g。以该方法对莱州湾海水养殖区内采集的野生鱼肌肉样品进行分析，共检出6种抗生素。该方法简便、快速、灵敏度高，为研究抗生素的暴露水平和环境行为奠定了基础。
A sample preparation and analytical method with accelerated solvent extraction ( ASE)and high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS)was developed to detect 19 antibiotic( 9 sulfonamides,4 quinolones,3 macrolides and 3 others) and 2 sulfonamide metabolite residues in fish muscle. The target compounds were extracted using ASE and purified simultaneously by a C18 resin in the extraction cell. The extracts were evaporated to dryness,and redissolved with the initial mobile phase for HPLC-MS/MS analysis after freezing centrifugation( 10 000 r/min,-4 ℃)to remove the fat and other matrix compounds further. The separation of the analytes was carried out on an Xterra MS C18 column with methanol-acetonitrile(1:1,v/v)as mobile phase A and 0. 1% formic acid(contai-ning 0. 1% ammonium formate)as mobile phase B. The spiked recoveries of the method were 55. 2%-113. 3%,with the relative standard deviations of 0. 1%-17. 6%( n=6 ). The limits of detection ranged from 0. 003 to 0. 6 ng/g. The method was applied to two fish( Synechogobius hasta and Liza haematocheilus)collected in mariculture areas of Laizhou Bay and six antibiot-ics were detected,in which the mass concentrations of norfloxacin were highest with mean values of 67. 01 and 27. 58 ng/g,respectively. The method is simple,rapid,highly sensitive, and useful in the study on exposure levels and environmental behavior of the antibiotics.
参考文献
| [1] | 李再兴;田宝阔;左剑恶.[J].环境工程,201230(02):72. |
| [2] | Food and Agriculture Organization of the United Nations (FAO).The State of World Fisheries and Aquaculture 2012[M].Rome:FAO Fisheries and Aquaculture Department,2012:27. |
| [3] | 王丹;隋倩;赵文涛.[J].科学通报,201459(09):743. |
| [4] | Gao P P;Mao D Q;Luo Y.[J].Water Res,201246(07):2355. |
| [5] | Willmott A;McCombie A;Rossleigh M.[J].Intern Med J,201141(Suppl 3):25. |
| [6] | 孙伟红;冷凯良;王志杰.[J].食品科学,200930(24):294. |
| [7] | Zhou Q;Peng D P;Wang Y L.[J].Food Chem,2014154:52. |
| [8] | Yu H;Tao Y F;Chen D M.[J].J Chromatogr B,2012885:150. |
| [9] | Tao Y F;Yu G;Chen D M.[J].J Chromatogr B,2012897:64. |
| [10] | Gentili A;Perret D;Marchese S.[J].J Agric Food Chem,200452(15):4614. |
| [11] | 杨常青;王龙星;侯晓虹.[J].色谱,201230(08):756. |
| [12] | 孟娟;杨永红.[J].中国食品卫生杂志,201224(06):546. |
| [13] | 龚强;丁利;朱绍华.[J].色谱,201230(11):1143. |
| [14] | Ding Y J;Zhang W H;Gu C.[J].J Chromatogr A,20111218(01):10. |
| [15] | 厉文辉;史亚利;高立红.[J].分析测试学报,201029(10):987. |
| [16] | 赵恒;孟祥周;向楠.[J].环境化学,201231(05):573. |
| [17] | Zhu L Y;Hites R A.[J].Environ Sci Technol,200640(12):3711. |
| [18] | IUPAC.[J].Pure Appl Chem,197645(02):107. |
| [19] | Runnqvist H;Bak S A;Hansen M.[J].J Chromatogr A,20101217(16):2447. |
| [20] | Carretero V;Blasco C;Picó Y.[J].J Chromatogr A,20081209(1/2):162. |
| [21] | Pecorelli I;Galarini R;Bibi R.[J].Anal Chim Acta,2003483(1/2):81. |
| [22] | Na G S;Fang X D;Cai Y Q.[J].Mar Pollut Bull,201369(1/2):233. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%