在线固相萃取-高效液相色谱-串联质谱法同时测定家禽养殖废水中6种抗菌类药物的残留量  

Simultaneous Determination of Residues of 6 Antibacterial Drugs in Poultry Breeding Wastewater by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Online Solid Phase Extraction

作　　者：宁方尧[1] 何善廉 温韬 NING Fangyao;HE Shanlian;WEN Tao(Guangxi Industrial Vocational and Technical College,Nanning 530000,China;Guangxi Zhuang Autonomous Region Product Quality Inspection Research Institute,Nanning 530000,China)

机构地区：[1]广西工业职业技术学院,南宁530000 [2]广西壮族自治区产品质量检验研究院,南宁530000

出　　处：《理化检验(化学分册)》2025年第4期407-411,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了在线固相萃取-高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定家禽养殖废水中6种抗菌类药物(氟苯尼考、磺胺甲基嘧啶、痢菌净、氟哌酸、阿米卡星和头孢唑林钠)残留量的方法。取家禽养殖废水样品用纱布过滤,再用滤纸过滤,取滤液10.0 m L,通过Waters Oasis HLB固相萃取柱在线固相萃取,以Capcell PAK AG ODS C18色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合液为流动相进行梯度洗脱,采用电喷雾离子(ESI)源,在正离子(ESI+)扫描模式下进行多反应监测(MRM)模式质谱分析。结果表明,6种抗菌类药物的质量浓度在0.005~5.0 mg·L^(-1)内与对应的峰面积呈线性关系,检出限(3S/N)为0.018 3~0.072 2μg·L^(-1)。按照标准加入法进行回收试验,回收率为83.8%~105%,测定值的相对标准偏差(n=6)均小于5.0%。方法用于测定5个实际家禽养殖废水中6种抗菌类药物的残留量,检出量为16.09~277.14μg·L^(-1)。A method for simultaneous determination of residues of 6 antibacterial drugs including flufenicol,sulfamethoxazole,carbendazim,norfloxacin,amikacin,and cefazolin sodium in poultry breeding wastewater by high performance liquid chromatography-tandem mass spectrometry with online solid phase extraction was proposed.The poultry breeding wastewater sample was taken and passed through gauze and filter paper.10.0 mL of the filtrate was taken and performed online solid phase extraction using Waters Oasis HLB solid phase extraction column.Capcell PAK AG ODS C18 column was used as the stationary phase and the mixed solution composed of 0.1%(volume fraction)formic acid solution and acetonitrile at different volume ratios was used as the mobile phase for gradient elution.Electrospray ion(ESI)source was used for mass spectrometry.The targets were analyzed by multiple reaction monitoring(MRM)mode in positive ion(ESI+)scanning mode.As shown by the results,linear relationships between the corresponding peak areas and mass concentrations of 6 antibacterial drugs were found within 0.005-5.0 mg·L^(-1),with detection limits(3S/N)in the range of 0.0183-0.0722μg·L^(-1).Test for recovery was made by the standard addition method,giving results in the range of 83.8%-105%,with RSDs(n=6)of the determined values less than 5.0%.This method could be used to determine the residues of 6 antibacterial drugs in 5 actual poultry breeding wastewater,and the detection amounts were in the range of 16.09-277.14μg·L^(-1).

关 键 词：在线固相萃取 高效液相色谱-串联质谱法(HPLC-MS/MS) 家禽养殖废水 抗菌类药物 

分 类 号：O657.63[理学—分析化学]