超高效液相色谱-串联质谱同时测定畜禽粪便发酵沼液中9种磺胺类抗生素
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S141;X502

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沈阳市科技计划项目(21-108-9-37);辽宁省教育厅科学研究经费项目(LSNJC202002);辽宁省自然科学基金(20180550984)


Simultaneous Determination of Nine Sulfonamides Antibiotics in Biogas Slurry Livestock and Poultry Manure by Ultra Performance Liquid ChromatographyTandem Mass Spectrometry
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    摘要:

    本文利用超高效液相色谱-串联质谱(UPLC-MS/MS)技术研究建立了同时测定畜禽粪便发酵沼液中9种磺胺类兽用抗生素残留的分析方法。样品经Na2EDTA提取,Oasis HLB固相萃取柱净化,采用电喷雾正电离源(ESI+)和选择性反应监测(MRM)模式进行检测,外标法定量。结果表明:9种磺胺类抗生素药物在0.01~5.0μg/mL质量浓度范围内与色谱峰面积线性拟合曲线的相关系数(r)均大于等于0.998 4,在0.01、0.05、0.5、2.0 mg/L 4个加标水平下平均回收率为62.3%~93.1%,相对标准偏差为3.64%~10.90%,检出限为0.1~0.8μg/L,定量下限为0.3~2.6μg/L。该方法净化效果显著、灵敏度高、重现性好,适用于畜禽粪便发酵沼液中9种磺胺类兽用抗生素残留的测定。

    Abstract:

    A method for the analysis of nine sulfonamides antibiotics residues in biogas slurry was established by using ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The samples were extracted by Na2EDTA. Liquid extract was purified by an Oasis HLB SPE column, Electrospray ionization(ESI+) and selective reaction monitoring(MRM) mode were used to detect and quantify by external standard method. The results showed that the Correlation Coefficient between the concentration range of 0.01-5.0 μg/mL, the linear curve of chromatographic peak area of 9 sulfonamide drugs were all greater than 0.9984, at the levels of 0.01, 0.05, 0.5, 2.0μg/L, the average recovery of the samples were 62.3%-93.1%, and the relative standard deviation was 3.64%-10.90%. The detection limit was 0.1-0.8 μg/L, and the limit of quantification(LOQ) was 0.3-2.6 μg/L. This method has good purification effect, high sensitivity and reproducibility. It is suitable for the determination of nine sulfonamides in biogas slurry.

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张敏,张杨开,徐宜宏,付海滨.超高效液相色谱-串联质谱同时测定畜禽粪便发酵沼液中9种磺胺类抗生素[J].东北农业科学,2022,47(5):120-123.

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  • 收稿日期:2020-03-13
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  • 在线发布日期: 2024-11-09
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