| 改良的QuEChERS/UPLC法测定鱼组织中磺胺甲唑、乙酰磺胺甲唑与甲氧苄啶 |
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| 基金项目:国家重点研发计划项目(2017YFC1600704)；现代农业产业技术体系专项资金资助项目(CARS-49)；中央级公益性科研院所基本科研业务费专项资金资助项目(2018JBF02) |
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| 中文摘要:建立了快速检测鱼体自然比例的带皮肌肉、肝脏、肾脏、鳃和血浆中磺胺甲唑(SMZ)及其代谢物乙酰磺胺甲唑(N-ac-SMZ)和增效剂甲氧苄啶(TMP)的超高效液相色谱法(UPLC)。自然比例的带皮肌肉、肝脏、肾脏和鳃组织采用改进的QuEChERS方法进行样品前处理；血浆样品采用液液萃取法进行前处理。以甲醇-01%乙酸水溶液为流动相，Acquity UPLC-BEH C18(2.1 mm×100 mm，1.7 μm)为分离柱，检测波长为270 nm，数据采集模式为吸光度-基线中值滤波(MBF)，外标法定量。结果表明，3种目标物在0.05~10 mg/L范围内线性良好，相关系数r2≥0.998 9，方法检出限和定量下限分别为25、50 μg/kg。在0.05~2.00 mg/kg加标水平下，回收率为68.2%~97.3%，相对标准偏差为1.7%~13%。该方法操作简便、准确、灵敏，适用于鱼体各组织中此3种目标物残留量的检测和药代动力学及组织分布规律研究。 |
| 中文关键词:改良的QuEChERS 磺胺甲唑 代谢物 甲氧苄啶 鱼组织 超高效液相色谱 |
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| Determination of Sulfamethoxazole,N-acetyl Sulfamethoxazole and Trimethoprim Residues in Fish Tissues by Ultra-high Performance Liquid Chromatography with Modified QuEChERS |
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| Abstract:An ultra high performance liquid chromatographic(UPLC) method was established for the rapid determination of sulfamethoxazole(SMZ),N acetyl sulfamethoxazole(N-ac-SMZ) and trimethoprim(TMP) in fish tissues,including muscle and skin in natural proportions,liver,kidney,gill and plasma.Samples of muscle and skin in natural proportions,liver,kidney and gill tissues of fish were prepared using the modified QuEChERS,and plasma sample was prepared by a liquid-liquid extraction procedure.The analytes were separated on an Acquity UPLC-BEH C18 column(2.1 mm×100 mm，1.7 μm) with methanol and water containing 0.1%acetic acid as mobile phases,at a detection wavelength of 270 nm,using an absorbent minus median baseline filter(MBF) in data acquisition mode.The external standard method was used for quantitation.Results showed that there were good linear relationships for SMZ,N ac-SMZ and TMP in the range of 0.05-10 mg/L with correlation coefficients(r2) not less than 0.998 9.The detection limits and quantitation limits for the analytes in fish tissues were 25 μg/kg and 50 μg/kg,respectively.Recoveries for the target compounds at spiked levels of 0.05-2.00 mg/kg were between 68.2%and 97.3%with relative standard deviations of 1.7%-13%.The method is simple,accurate and highly sensitive,and is suitable for the residue determination,pharmacokinetic and tissue distribution study of SMZ,N-ac-SMZ and TMP in fish. |
| Key Words:modified QuEChERS sulfamethoxazole metabolite trimethoprim fish tissue ultra high performance liquid chromatography(UPLC) |
| 引用本文：刘永涛,韩刚,宋金龙,董靖,胥宁,杨移斌,杨秋红,艾晓辉.改良的QuEChERS/UPLC法测定鱼组织中磺胺甲唑、乙酰磺胺甲唑与甲氧苄啶[J].分析测试学报,2019,38(8):973-978. |
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