爲探索一次性檢測豬肉中多種(zhǒ公工ng)磺胺類藥物殘留的檢測方法,公錢建立了同時(shí)測定豬肉中22種(zhǒng)磺胺類業女藥物殘留的固相萃取-超高效液相色譜方法。樣(yà要雜ng)品用3%乙酸乙腈提取,MCX固相萃取柱淨化,水和甲水術醇淋洗,5%氨化甲醇洗脫,氮氣吹至近幹,0.1%甲酸-乙腈(9:1身著,V/V)溶液複溶,二極管陣列檢測器計也270 nm檢測。結果顯示:該方法對(duì)22種(zhǒng)磺胺類藥物那兒檢測的線性關系良好(hǎo)(R2>0.999),定量限爲2.5~1快不0.0 μg/kg,檢測限爲1.0~4.0 μg頻文/kg;各藥物平均回收率爲83.2務也%~96.6%,批内和批間變異系數分别爲購民1.1%~3.5%和3.6%~13.4%。結果表明線坐,該方法靈敏度高、重複性好(hǎo)、成(chéng)本子厭低廉,且操作簡單、快速,可用于豬肉樣(yàng)品中多種(zhǒng黃化)磺胺類藥物殘留的同時(shí)檢測。
Simultaneous Determinati吧年on of 22 Kinds of Sulfonami相業de Residues in Pork by SPE-UPLC
In order to develop a method for simul通一taneously detecting va廠通rious sulfonamide r能訊esidues in pork,a solid-phase ex校我traction-ultra-high performance liqui吃睡d chromatography(SPE-UPLC)me兒水thod for detecting 紙藍22 kinds of sulfonamide residue暗信s in pork was established. Samples用錢 were extracted by 3北錯% acetic acid acetonitrile,purified b著報y MCX solid phase extract校場ion column,rinsed by water and西朋 methanol,eluted by 5% ammoniated meth短長anol,dried by blowing with nitrogen,拍冷and redissolved by 0.1% fo服區rmic acid-aceton錢就itrile(9:1,V/V)solu制員tion,and then detect鐵鐵ed by a diode array detector at 270 nm男短. The results showed that the linear車那 relationship was goo工也d(R2>0.999)for detect明河ion of the 22 kinds of s村來ulfonamides by the method,with the li物鄉mit of quantification of 2.5服綠 to 10.0 μg/kg,the detection 術司limit of 1.0 to行媽 4.0 μg/kg;the average很自 recovery rate of each drug ranged 83信大.2% to 96.6%,and the variable c技河oefficients within and between雜到 batches were 1.1% to 3.5% an科見d 3.6% to 13.4%,respectiv新跳ely. It was concluded that vario計民us sulfonamide 他分residues in pork could be simultaneou會男sly detected by the established m市要ethod due to its advantages 讀購of high sensitivity,good repeatability不著,low cost,simple a上數nd rapid operation.
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