王小乔, 李坚, 许晓辉, 李剑勇, 吴福祥, 张虹艳, 潘秀丽, 李赟. 分散固相萃取-超高效液相色谱-串联质谱法测定海龙中11种磺胺类抗菌药物残留[J]. 分析测试技术与仪器, 2023, 29(1): 16-22. DOI: 10.16495/j.1006-3757.2023.01.003
引用本文: 王小乔, 李坚, 许晓辉, 李剑勇, 吴福祥, 张虹艳, 潘秀丽, 李赟. 分散固相萃取-超高效液相色谱-串联质谱法测定海龙中11种磺胺类抗菌药物残留[J]. 分析测试技术与仪器, 2023, 29(1): 16-22. DOI: 10.16495/j.1006-3757.2023.01.003
WANG Xiaoqiao, LI Jian, XU Xiaohui, LI Jianyong, WU Fuxiang, ZHANG Hongyan, PAN Xiuli, LI Yun. Determination of 11 Sulfonamide Antibacterial Drug Residues in Syngnathus by Ultra-Performance Liquid Chromatography-Mass Spectrometry Combined with Dispersed Solid Phase Extraction[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 16-22. DOI: 10.16495/j.1006-3757.2023.01.003
Citation: WANG Xiaoqiao, LI Jian, XU Xiaohui, LI Jianyong, WU Fuxiang, ZHANG Hongyan, PAN Xiuli, LI Yun. Determination of 11 Sulfonamide Antibacterial Drug Residues in Syngnathus by Ultra-Performance Liquid Chromatography-Mass Spectrometry Combined with Dispersed Solid Phase Extraction[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 16-22. DOI: 10.16495/j.1006-3757.2023.01.003

分散固相萃取-超高效液相色谱-串联质谱法测定海龙中11种磺胺类抗菌药物残留

Determination of 11 Sulfonamide Antibacterial Drug Residues in Syngnathus by Ultra-Performance Liquid Chromatography-Mass Spectrometry Combined with Dispersed Solid Phase Extraction

  • 摘要: 采用超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)技术,建立了测定海龙中11种磺胺类抗菌药物残留量的分析方法. 样品经2%甲酸-乙腈超声提取,增强型脂质去除分散固相萃取净化管(EMR-Lipid dSPE)净化,采用Waters ACQUITY BEH C18色谱柱(1.7 μm,2.1 mm×100 mm)分离,电喷雾离子源电离,正离子多反应监测模式(MRM)检测,以含2 mmol/L乙酸铵-0.1%甲酸的水溶液和含0.1%甲酸的乙腈溶液为流动相进行梯度洗脱,外标法定量. 11种磺胺类抗菌药物在0~30 ng/mL的质量浓度范围内线性关系良好,相关系数(R2)均不低于0.995 9,检出限(LOD)与定量限(LOQ)分别在0.11~1.30 µg/kg和0.37~4.40 µg/kg之间,11种磺胺类抗菌药物在质量浓度为20.0、50.0、100.0 µg/kg时的三个加标水平的平均回收率为62.5%~118.1%,相对标准偏差为2.1%~9.2%. 方法前处理简便、准确性好,可用于海龙中11种磺胺类抗菌药物残留的快速筛查.

     

    Abstract: An analytical method for the determination of 11 sulfonamide antibacterial drug residues in Syngnathus by ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS) has been established. The samples were extracted by ultrasonication with 2% formic acid-acetonitrile, purified by an enhanced matrix removal lipid-dispersed solid phase extraction (EMR-Lipid dSPE), and separated on a Waters ACQUITY BEH C18 column (1.7 μm, 2.1 mm×100 mm). The analytes were detected by mass spectrometry using the positive electrospray ionization mode under multiple reaction monitoring mode (MRM), with 2 mmol/L ammonium acetate-0.1% formic acid in aqueous solution and 0.1% formic acid in acetonitrile as mobile phases by a gradient elution program, and quantified by the external standard method. The results showed that the 11 antibacterial sulfonamides had good linearity in the range of 0~30 ng/mL, the correlation coefficient (R2) were all greater than 0.9959, the limit of detection (LOD) and quantitation (LOQ) were in the range of 0.11~1.30 µg/kg and 0.37~4.40 µg/kg, respectively. At three spiked levels of 20.0, 50.0 and 100.0 µg/kg, the spiked average recoveries of the analytes were in the range of 62.5%~118.1%, and the relative standard deviation was 2.1%~9.2%. The method is accurate, straightforward, and is suitable for the rapid screening of 11 sulfonamide antibacterial drug residues in Syngnathus.

     

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