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    钱诗颖, 蓝雅琼, 刘倩, 司文帅, 孙明星, 王鲁梅, 沈国清. 响应面优化超高效液相色谱-串联质谱法同时测定有机肥中14种磺胺类抗生素[J]. 华东理工大学学报(自然科学版), 2021, 47(2): 209-216. DOI: 10.14135/j.cnki.1006-3080.20191115001
    引用本文: 钱诗颖, 蓝雅琼, 刘倩, 司文帅, 孙明星, 王鲁梅, 沈国清. 响应面优化超高效液相色谱-串联质谱法同时测定有机肥中14种磺胺类抗生素[J]. 华东理工大学学报(自然科学版), 2021, 47(2): 209-216. DOI: 10.14135/j.cnki.1006-3080.20191115001
    QIAN Shiying, LAN Yaqiong, LIU Qian, SI Wenshuai, SUN Mingxing, WANG Lumei, SHEN Guoqing. Response Surface Optimization of Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for Simultaneous Determination of 14 Kinds of Sulfonamide Antibiotics in Organic Fertilizers[J]. Journal of East China University of Science and Technology, 2021, 47(2): 209-216. DOI: 10.14135/j.cnki.1006-3080.20191115001
    Citation: QIAN Shiying, LAN Yaqiong, LIU Qian, SI Wenshuai, SUN Mingxing, WANG Lumei, SHEN Guoqing. Response Surface Optimization of Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for Simultaneous Determination of 14 Kinds of Sulfonamide Antibiotics in Organic Fertilizers[J]. Journal of East China University of Science and Technology, 2021, 47(2): 209-216. DOI: 10.14135/j.cnki.1006-3080.20191115001

    响应面优化超高效液相色谱-串联质谱法同时测定有机肥中14种磺胺类抗生素

    Response Surface Optimization of Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for Simultaneous Determination of 14 Kinds of Sulfonamide Antibiotics in Organic Fertilizers

    • 摘要: 建立了一种超高效液相色谱-串联质谱(UHPLC-MS/MS)同时测定有机肥中14种磺胺类抗生素的方法。在明确最佳提取溶剂条件为乙腈与乙酸体积比为80∶20的基础上,采用Box-Behnken Design方法设计实验,对前处理中缓冲液体积、缓冲液pH和振荡时间3个参数进行响应面优化。结果表明,在提取液中加入6.15 mL的乙二胺四乙酸二钠(Na2EDTA)-Mcllvaline缓冲液(pH 3.0),振荡时间为20 min时,14种抗生素的平均提取回收率达到69.31%~76.39%。对优化后的前处理方法进行验证,相对标准偏差(RSD)小于3.04 %,表明该方法重现性较好。

       

      Abstract: Sulfonamides (SAs) are frequently used as feed additives to prevent and treat animal diseases because of their low cost, high stability and strong hydrophilicity. However, the incomplete adsorption of SAs in the living body makes them excreted in the form of derived products or original structures. These excrements can bring serious pollution in soil when being used as manures. Therefore, more and more attention has been paid for the detection of antibiotics in organic fertilizer in recent years. In this study, a method for the simultaneous determination of 14 kinds of sulfonamide antibiotics in organic fertilizers by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. The samples were purified and concentrated by MCX solid phase extraction column after mixing with extraction solution. Methanol, ammonium acetate (10 mmol/L) and formic acid aqueous solution (0.1%, mass fraction) were used as mobile phases. The samples after pretreatment were separated by gradient elution and analyzed qualitatively under UHPLC-MS/MS multi-reaction monitoring mode. The effects of different kinds of extraction solvents on extraction efficiency during pretreatment were compared. When acetonitrile/acetic acid (volume ratio: 80/20) was used as the extraction solvents, the average recovery of 14 sulfonamide antibiotics was 53.78%—90.29%. Box-Behnken design, a kind of responsive surface methodology, was used to optimize the three parameters of buffer volume, buffer pH and oscillation time to enhance the average recovery of 14 sulfonamide antibiotics. Under the optimal extraction conditions (6.15 mL Na2EDTA-Mcllvaline buffer, pH 3.0 and 20 min of the oscillation time), the average recovery of 14 antibiotics was 69.31%—76.39%. The relative standard deviation (RSD) of the optimized pretreatment method was less than 3.04%, which indicated that the method had good reproducibility and could be applied to the determination and analysis of actual samples.

       

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