為探索一次性檢測豬肉中多種磺胺類藥物殘留的檢測方法，建立了同時測定豬肉中22種磺胺類藥物殘留的固相萃取-超高效液相色譜方法。樣品用3%乙酸乙腈提取，MCX固相萃取柱凈化，水和甲醇淋洗，5%氨化甲醇洗脫，氮氣吹至近干，0.1%甲酸-乙腈（9:1，V/V）溶液復溶，二極管陣列檢測器270 nm檢測。結(jié)果顯示：該方法對22種磺胺類藥物檢測的線性關(guān)系良好（R2＞0.999），定量限為2.5~10.0 μg/kg，檢測限為1.0~4.0 μg/kg；各藥物平均回收率為83.2%~96.6%，批內(nèi)和批間變異系數(shù)分別為1.1%~3.5%和3.6%~13.4%。結(jié)果表明，該方法靈敏度高、重復性好、成本低廉，且操作簡單、快速，可用于豬肉樣品中多種磺胺類藥物殘留的同時檢測。
Simultaneous Determination of 22 Kinds of Sulfonamide Residues in Pork by SPE-UPLC
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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