國家獸藥產(chǎn)業(yè)技術(shù)創(chuàng)新聯(lián)盟 National veterinary drug industry technology innovation alliance |
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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(fù)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(fù)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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國家獸藥產(chǎn)業(yè)技術(shù)創(chuàng)新聯(lián)盟 National veterinary drug industry technology innovation alliance |
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