分析测试学报2012,Vol.31Issue(3):302-306,5.DOI:10.3969/j.issn.1004-4957.2012.03.011
畜禽粪便中的氟喹诺酮类与四环素类兽药残留同时提取的方法研究
Study on Simultaneous Extraction of Fluoroquinolones (FQs) and Tetracyclines (TCs) in Manure
摘要
Abstract
The extraction effects of fluoroquinolones ( FQs) and tetracyclines ( TCs) in manure were compared experimantally by using different extractions, and the method of mixed extractions of EDTA - Mcllvaine and 50% Mg( NO3 )2 - 2. 5% NH3 · H2O was developed. The proportion of two extractions was explored. The result indicated that when the volume ratio of EDTA - Mcllvaine and 50% Mg(NO3)2 -2. 5% NH3 · H20 was 3:1, the extraction ratios for the six antibiotics, including tetracycline (TC) , chlortetracy ( CTC ) , enrofloxacin ( ENR) , pefloxacin ( PEF) , danofloxain (DAR) and sarafloxacin(SAR) were between 84% and 92% . Based on this, the methods of solid phase extraction and purification for the six residued drugs were optimized through the investigation on different elution-volume and extraction columns. At the same time, the concentration method was established by optimizing the conditions that using nitrogen concentration and rotation-evaporation. E-ventually, the simultaneous extraction and determination of fluoroquinolones ( FQs) and tetracyclines (TCs) in manure by high performance capillary electrophoresis( HPCE) was established. Under the optimal chromatographic conditions, the linear ranges were between 3. 125 mg/L and 100 mg/L, the limit of quantitation for six antibiotics were less than 0. 1 mg/kg. At the spiked concentrations of 10.0, 20.0, 40. 0 mg/L, recoveries of six antibiotics in manure ranged from 54% to 93% with relative standard deviations(RSDs) of 6. 3% - 8. 9% . This method was quite simple, rapid and lowcost, and was successfully used in the detection of six antibiotics in manure around the city of Hefei.关键词
粪便/前处理/氟喹诺酮/四环素/高效毛细管电泳/同时提取Key words
manure/ pretreatment/ fluoroquinolones/ tetracyclines/ high performance capillary e-lectrophoresis(HPCE) / simultaneous extraction分类
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沈虎琴,檀华蓉,祁克宗,田春秋..畜禽粪便中的氟喹诺酮类与四环素类兽药残留同时提取的方法研究[J].分析测试学报,2012,31(3):302-306,5.基金项目
“十一·五”国家科技支撑项目( 2006 BAK02 A08_4) ( 2006 BAK02 A08_4)