摘要:
建立了蔬菜中四环素类抗生素(TCs)的固相萃取-高效液相色谱-荧光检测(HPLC-FLD)分析方法.蔬菜样品以(乙腈+Na2SO4+CH3COONa+Na2EDTA+CaCl2)溶液超声提取,提取液再用正己烷进行液-液萃取去脂,以HLB柱净化富集.利用HPLC-FLD,以缓冲液[0.35mol·l-1CaCl2 +0.025mol·l-1Na2EDTA+0.075mol·l-1CH3COONa(pH=7.3)]-乙腈(82.5:17.5,V/V)为流动相,于激发波长390nm、发射波长512nm处进行检测.蔬菜样品中土霉素(OTC)和四环素(TC)的定量限分别为0.471μg·kg-1和0.532μg·kg-1,加标回收率为68.61%—114.12%.利用该方法对不同蔬菜样品的分析结果表明,OTC和TC的含量分别在0.041—0.174mg·kg-1(鲜重)和0—0.048mg·kg-1(鲜重)之间,部分蔬菜中OTC的含量高于我国农业部动物性食品中控制标准.
Abstract:
An analytical method for the detemination of tetracycline antibiotics in vegetable using solid phase extraction and high performance liquid chromatography(HPLC)with fluorescence detection was developed and validated,which is effective and low-cost.Samples were extracted by acetonitrile(adding sodium sulfate,sodium acetate,disodium ethylenediam-inetetraacetate and calcium chloride)with ultrasonic processing,defatted by a double liquid liquid extraction with n-hexane,then purified and enriched by the HLB cartridges.Analytes were detected using acetonitrile and 0.35mol·l-1 CaCl2 、0.025mol·l-1 Na2EDTA、0.075mol·l-1 CH3COONa pH=7.3(82.5:17.5,V/V)as the mobile phase,with fluorescence detection at 390 nm excitation and 512 nm emission,The quantitative limit of vegetable samples for OTC and TC were 0.471 and 0.532 μg·kg-1,respectively.The recoveries of different additional doses were 68.61% to 114.12%.The method was applied to determine the practical vegetable samples.The concentrations of OTC and TC in vegetable samples ranged from 0.041 to 0.174 mg·kg-1(FW)and from 0 to 0.048 mg·kg-1(FW),respectively.
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