加速溶剂萃取-高效液相色谱-串联质谱联用测定莱州湾海水养殖区野生鱼肌肉中19种抗生素及2种磺胺代谢产物残留

Determination of 19 antibiotic and 2 sulfonamide metabolite residues in wild fish muscle in mariculture areas of Laizhou Bay using accelerated solvent extraction and high performance liquid chromatography-tandem mass spectrometry

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 3others）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 oth er 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（containing 0. 1% ammonium formate）as mobile phase B. The spiked recoveries of the meth od 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（Syne chogobius hasta and Liza haematocheilus）collected in mariculture areas of Laizhou Bay and six antibiotics 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 sensi tive,and useful in the study on exposure levels and environmental behavior of the antibiotics.