固相萃取-超高效液相色谱法同时测定猪肉中22种磺胺类药物残留
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S859.8

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Simultaneous Determination of 22 Kinds of Sulfonamide Residues in Pork by SPE-UPLC
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    摘要:

    为探索一次性检测猪肉中多种磺胺类药物残留的检测方法,建立了同时测定猪肉中22种磺胺类药物残留的固相萃取-超高效液相色谱方法。样品用3%乙酸乙腈提取,MCX固相萃取柱净化,水和甲醇淋洗,5%氨化甲醇洗脱,氮气吹至近干,0.1%甲酸-乙腈(9:1,V/V)溶液复溶,二极管阵列检测器270 nm检测。结果显示:该方法对22种磺胺类药物检测的线性关系良好(R2>0.999),定量限为2.5~10.0 μg/kg,检测限为1.0~4.0 μg/kg;各药物平均回收率为83.2%~96.6%,批内和批间变异系数分别为1.1%~3.5%和3.6%~13.4%。结果表明,该方法灵敏度高、重复性好、成本低廉,且操作简单、快速,可用于猪肉样品中多种磺胺类药物残留的同时检测。

    Abstract:

    In order to develop a method for simultaneously detecting various sulfonamide residues in pork,a solid-phase extraction-ultra-high performance liquid chromatography(SPE-UPLC)method for detecting 22 kinds of sulfonamide residues in pork was established. Samples were extracted by 3% acetic acid acetonitrile,purified by MCX solid phase extraction column,rinsed by water and methanol,eluted by 5% ammoniated methanol,dried by blowing with nitrogen,and redissolved by 0.1% formic acid-acetonitrile(9:1,V/V)solution,and then detected by a diode array detector at 270 nm. The results showed that the linear relationship was good(R2>0.999)for detection of the 22 kinds of sulfonamides by the method,with the limit of quantification of 2.5 to 10.0 μg/kg,the detection limit of 1.0 to 4.0 μg/kg;the average recovery rate of each drug ranged 83.2% to 96.6%,and the variable coefficients within and between batches were 1.1% to 3.5% and 3.6% to 13.4%,respectively. It was concluded that various sulfonamide residues in pork could be simultaneously detected by the established method due to its advantages of high sensitivity,good repeatability,low cost,simple and rapid operation.

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王宏宇,武云龙,赵栋皓,孙晓亮,李木子,曹旭敏,宋翠平,赵思俊,李存.固相萃取-超高效液相色谱法同时测定猪肉中22种磺胺类药物残留[J].《中国动物检疫》编辑部,2021,38(7):105-111.

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