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