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

实验比较了不同提取剂对养殖场畜禽粪便中喹诺酮类与四环素类6种兽药残留的提取效果,确定以EDTA-McIlvaine与50%Mg(NO3)2-2.5%NH3.H2O混合液进行提取,并考察了两种提取剂混合比例的影响。结果表明,当EDTA-McIlvaine与50%Mg(NO3)2-2.5%NH3.H2O提取剂的体积比为3∶1时,6种兽药残留的提取率为84%～92%。在此基础上,考察了不同洗脱液体积、萃取小柱的影响,优化了6种兽药残留的固相萃取纯化方法,比较了氮吹仪与旋转蒸发的浓缩方法,建立了高效毛细管电泳同时检测畜禽粪便中氟喹诺酮类与四环素类兽药残留的方法。在优化的电泳条件下,方法的线性范围为3.125～100 mg/L,6种药物的定量下限均小于0.1 mg/kg;在10.0、20.0、40.0 mg/L的加标水平下,四环素、金霉素、恩诺沙星、达氟沙星、培氟沙星、沙拉沙星的回收率为54%～93%,相对标准偏差(RSD)为6.3%～8.9%。该方法简便、快速、成本低,已成功用于合肥市周边地区畜禽粪便中兽药残留的检测。

Study on Simultaneous Extraction of Fluoroquinolones(FQs) and Tetracyclines(TCs) in Manure

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-McIlvaine 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-McIlvaine and 50% Mg(NO3)2-2.5% NH3·H2O 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.Eventually,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 low-cost,and was successfully used in the detection of six antibiotics in manure around the city of Hefei.