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出 处:《粮食与饲料工业》2016年第1期72-75,共4页Cereal & Feed Industry
摘 要:研究了以本体聚合法制备的喹乙醇分子印迹聚合物作为固相萃取填充材料,建立了分子印迹固相萃取与高效液相色谱联用技术检测饲料中残留痕量喹乙醇的方法。通过优化分子印迹固相萃取条件,确定用0.5ml甲醇-水(90∶10,V/V)洗脱液,在上样流速为1.2ml/min,样品在pH7~8条件下,对喹乙醇有较好富集效果。为了评价分子印迹固相萃取材料对模板分子喹乙醇的选择富集能力,分别以分子印迹聚合物和C18为固相萃取填充柱比较富集效果。在上样流速为1.2ml/min条件下,预富集42min,分子印迹固相萃取材料富集倍数达78,最低检测限(S/N=3)为88.0ng/L,连续在线富集5次的精密度(相对标准偏差)为4.6%。对添加有喹乙醇浓度为0.002 5和0.010 0mg/g的饲料进行检测,其添加回收率为89.5%和93.4%。The molecularly imprinted polymers was synthesized by bulk polymerization using olaquindox as template molecule. A method for determination of olaquindox in feed using molecularly imprinted solid-phase extraction (MISPE) coupied to high-performance liquid chromatography was presented. By optimizing the molecularly imprinted solid phase extraction condition, the determine conditions with 0.5 ml of methanol/water (90 :10, v/v) eluent, the sample flow rate of 1.2 ml/min, sample pH within 7 to 8, have good concentration effect of olaquindox. To evaluate molecularly imprinted solid phase extraction enrichment ability and seIection of template molecules, the enrichment effect to olaquindox respectively with molecularly imprinted polymer and C18 as packed column in solid phase extraction was conducted. With a loading flow rate of 1.2 ml/min, an enrichment factor of 78 was achieved. Under the selected MISPE condition, the detection limit (S/N= 3) for olaquindox was 88.0 ng/L, the RSD for five replicate extractions was 4.6%. The blank chicken samples spiked with olaquindox at 0. 002 5 and 0. 010 0 mg/g levels were extracted and determined by the developed method with recoveries of 89.5% and 93.4%, respectively.
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