固相萃取-液相色谱-串联质谱法快速测定猪肉中27种兽药及代谢物残留量  

Simultaneous determination of 27 kinds of veterinary drugs and their metabolites in swine meat by liquid chromatography-tandem mass spectrometry with solid phase extraction

作　　者：孙梅梅 吴银良 SUN Mei-Mei;WU Yin-Liang(Academy of Ningbo Agricultural Sciences,Ningbo 315040,China;Ningbo Key Laboratory for Testing and Control for Characteristic Agro-product Quality and Safety,Ningbo 315040,China)

机构地区：[1]宁波市农业科学研究院,宁波315040 [2]宁波市特色农产品质量安全检测与控制重点实验室,宁波315040

出　　处：《食品安全质量检测学报》2024年第17期30-38,共9页Journal of Food Safety and Quality

基　　金：浙江省“领雁”研发攻关项目(2022C02028)。

摘　　要：目的建立固相萃取-液相色谱-串联质谱法快速测定猪肉中27种兽药(磺胺类、喹诺酮类及苯并咪唑类药物)及代谢物残留量的分析方法。方法匀质后的猪肉样品用80%乙腈溶液提取,提取后用EMR-Lipid固相萃取小柱净化,流出液直接进行上机测定,采用ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,以0.1%甲酸溶液(含5mmol/L乙酸铵)和乙腈作为流动相进行梯度洗脱,电喷雾正离子模式下监测,内标法定量。结果27种化合物在0.075~50.000μg/L范围内线性关系良好,相关系数(r^(2))均高于0.9980,方法检出限和定量限分别为0.06~0.30μg/kg和0.20~1.00μg/kg。27种兽药及代谢物在1.0、10.0和100.0μg/kg添加浓度水平下平均添加回收率为88.5%~104.0%,相对标准偏差为2.6%~8.0%。结论该方法准确度和灵敏度高,前处理简单快速,适用于猪肉中磺胺类药物、喹诺酮类药物及苯并咪唑类药物的同时分析。Objective To establish a simple and fast analytical method for simultaneous determination of residues of 27 kinds of veterinary drugs(sulfonamides,quinolones,and benzimidazoles)and their metabolites in swine meat by liquid chromatography-tandem mass spectrometry with solid phase extraction.Methods The homogenized meat samples were extracted with 80%acetonitrile solution.After extraction,a solid phase extraction procedure was carried out with EMR-Lipid cartridge without activation procedure.Then,the effluent was collected and directly used for chromatographic separation on an ACQUITY UPLC HSS T3 column with a gradient elution of 0.1%formic acid in water with 5 mmol/L ammonium acetate/acetonitrile.The compounds were monitored in electrospray positive ion mode and quantified by internal standard method.Results Good linear relationship had been obtained ranging from 0.075 to 50.000μg/L for the 27 kinds of veterinary drugs and their metabolites,and the correlation coefficients(r^(2))were higher than 0.9980.The limits of detection and quantification were 0.06–0.30μg/kg and 0.20–1.00μg/kg,respectively.The average recoveries of 27 kinds of veterinary drugs and metabolites were 88.5%–104.0%and the relative standard deviations were 2.6%–8.0%at the concentrations of 1.0,10.0 and 100.0μg/kg.Conclusion The method has high accuracy and sensitivity,simple and fast pre-treatment,and is suitable for the simultaneous analysis of sulfonamides,quinolones and benzimidazoles in swine meat.

关 键 词：猪肉 磺胺类药物 喹诺酮类药物 苯并咪唑类药物 固相萃取 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS251.51[理学—化学]