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中国精品科技期刊2020
谢瑜杰,李铁梅,牛相涛,等. 一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留[J]. 食品工业科技,2021,42(20):268−278. doi: 10.13386/j.issn1002-0306.2021010156.
引用本文: 谢瑜杰,李铁梅,牛相涛,等. 一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留[J]. 食品工业科技,2021,42(20):268−278. doi: 10.13386/j.issn1002-0306.2021010156.
XIE Yujie, LI Tiemei, NIU Xiangtao, et al. Determination of Sulfonamides in Beef by One Step QuEChERS Method Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(20): 268−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010156.
Citation: XIE Yujie, LI Tiemei, NIU Xiangtao, et al. Determination of Sulfonamides in Beef by One Step QuEChERS Method Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(20): 268−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010156.

一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留

Determination of Sulfonamides in Beef by One Step QuEChERS Method Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了一种基于一步式QuEChERS自动提取和净化的技术,结合高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时检测牛肉中25种磺胺类药物残留的检测方法。样品经1%乙酸-乙腈提取,以C18、PSA和无水硫酸镁为净化吸附剂,采用一步式QuEChERS自动化前处理设备提取、净化、离心,经C18色谱柱进行分离,以0.2%甲酸甲醇−0.2%甲酸水(含2 mmol/L乙酸铵)为流动相梯度洗脱,ESI正离子模式扫描,多反应监测(Multi-reaction monitoring, MRM)测定,外标法定量。结果表明,所有化合物在0.1~20 μg/L的浓度范围内线性关系良好,相关系数不低于0.990,检出限(LOD)为0.1~3 μg/kg,定量限(LOQ)为1~10 μg/kg。在1、2和10倍LOQ三个加标浓度水平下,目标化合物的平均回收率范围为70.14%~116.93%,相对标准偏差(RSD)范围为0.95%~13.74%(n=5)。该方法简单快速、准确可靠、可用于检测牛肉中磺胺类药物的残留。

     

    Abstract: The method for simultaneous determination of 25 sulfonamides residues in beef was established by one-step automatic extraction and purification technology of QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with 1% acetonitrile acetate, C18, PSA and anhydrous magnesium sulfate were used as purification adsorbents, and the one-step QuEChERS automatic pretreatment equipment was used for extraction, purification and centrifugation. The analytes were separated by a reversed phase C18 column and eluted with 0.2% formic acid methanol and 0.2% formic acid water (containing 2 mmol/L ammonium acetate). The beef sample was analyzed under the multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+) and quantify by external standard. The results showed that good linearities were obtained for the 25 sulfonamides in 0.1~20 μg/L with the linear correlation coefficients more than 0.990. The limits of detection (LOD) and the limits of quantification (LOQ) for sulfonamides were 0.1~3 μg/kg and 1~10 μg/kg, respectively. The recoveries at three levels were in the range of 70.14%~116.93%. The repeatability expressed as relative standard deviations (RSD) was ranged from 0.95% to 13.74%(n=5). The method was simple, rapid, accurate and reliable, and could be used to detect the residues of sulfonamides in beef.

     

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