食品研究与开发
食品研究與開髮
식품연구여개발
Food Research and Development
2015年
20期
152-155
,共4页
氟喹诺酮类药物%固相萃取%高效液相色谱%检测
氟喹諾酮類藥物%固相萃取%高效液相色譜%檢測
불규낙동류약물%고상췌취%고효액상색보%검측
fluoroquinolones%SPE%HPLC%detection
以3种氟喹诺酮类抗菌药物-诺氟沙星、环丙沙星,恩诺沙星为研究对象,结合固相萃取串联高效液相色谱,建立动物源性食品中3种分析物残留的准确、灵敏的分析方法。研究采用Cleanert S C18固相萃取小柱为基质净化柱,以Hypersil-ODS C18柱(4.6 mm ×250 mm)为液相分离柱,0.05 mol/L H3PO4-三乙胺溶液(pH 2.4)∶乙腈为82∶18(体积比)为流动相,流速0.8 mL/min,能够达到基质净化和分析物富集、分离目的。根据实验结果,所建立的方法对3种氟喹诺酮类药物的最低检出限分别达到1.5、1.3、1.5μg/L;对3个添加浓度下的鸡肉、鸡蛋、牛奶和牛肉等复杂食品样品中3种分析物残留的检测也具有较高的准确度(回收率>90.0%)和重现性(RSD<5.0%,n=3)。
以3種氟喹諾酮類抗菌藥物-諾氟沙星、環丙沙星,恩諾沙星為研究對象,結閤固相萃取串聯高效液相色譜,建立動物源性食品中3種分析物殘留的準確、靈敏的分析方法。研究採用Cleanert S C18固相萃取小柱為基質淨化柱,以Hypersil-ODS C18柱(4.6 mm ×250 mm)為液相分離柱,0.05 mol/L H3PO4-三乙胺溶液(pH 2.4)∶乙腈為82∶18(體積比)為流動相,流速0.8 mL/min,能夠達到基質淨化和分析物富集、分離目的。根據實驗結果,所建立的方法對3種氟喹諾酮類藥物的最低檢齣限分彆達到1.5、1.3、1.5μg/L;對3箇添加濃度下的鷄肉、鷄蛋、牛奶和牛肉等複雜食品樣品中3種分析物殘留的檢測也具有較高的準確度(迴收率>90.0%)和重現性(RSD<5.0%,n=3)。
이3충불규낙동류항균약물-낙불사성、배병사성,은낙사성위연구대상,결합고상췌취천련고효액상색보,건립동물원성식품중3충분석물잔류적준학、령민적분석방법。연구채용Cleanert S C18고상췌취소주위기질정화주,이Hypersil-ODS C18주(4.6 mm ×250 mm)위액상분리주,0.05 mol/L H3PO4-삼을알용액(pH 2.4)∶을정위82∶18(체적비)위류동상,류속0.8 mL/min,능구체도기질정화화분석물부집、분리목적。근거실험결과,소건립적방법대3충불규낙동류약물적최저검출한분별체도1.5、1.3、1.5μg/L;대3개첨가농도하적계육、계단、우내화우육등복잡식품양품중3충분석물잔류적검측야구유교고적준학도(회수솔>90.0%)화중현성(RSD<5.0%,n=3)。
An accurate and sensitive method for the detection of three fluoroquinolones-norfloxacin (NOR), ciprofloxacin (CIPRO), enrofloxacin (ENRO) residues in animal-derived food products was developed by combining solid-phase extraction with high performance liquid chromatography. The Cleanert S C18 solid-phase extraction column was used for complex matrix purification and one Hypersil-ODS C18 column (4.6 mm × 250 mm) was employed for separation in liquid chromatography. The mobile phase consisted of 0.05 mol/L H3PO4 was controlled pH at 2.4 by triethylamine and mixed with ACN at the ratio of 82∶18 (volume ratio), and the flow rate controlled at 0.8 mL/min for the purpose of obtaining good substrate clean-up and analytes enrichment. Based on the obtained resluts, the detection limit of three chosen analytes achieved to 1.5 μg/L (NOR),1.3μg/L (CIPRO),1.5μg/L (ENRO) in the developed method, good recoveries in chosen chicken muscle, egg, milk and beef samples at three spiked levels of NOR, CIPRO and ENRO were obtained higher than 90.0 %with RSD less than 5.0%(n=3), meaning that the developed method in this research was high accuracy and reproducibility.