超声辅助离子液体冷诱导微萃取法测定肉类中氟甲喹和萘啶酸
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摘要
建立了一种样品前处理方法即离子液体冷诱导微萃取,通过超声辅助利用高效液相色谱-紫外检测器测定了鸡肉、猪肉中氟甲喹和萘啶酸的残留含量。考察了萃取剂、抗黏剂、pH值及温度等对萃取效率的影响。在优化的萃取条件下,测定氟甲喹和萘啶酸的线性范围分别为10～300μg·L~(-1)和5-300μg·L~(-1),r=0.9995及0.9997,检出限分别为0.7μg·L~(-1)和0.5μg·L~(-1),平均回收率在90.4%～103.2%,相对标准偏差在2.7%～9.3%之间。本方法具有简单、环保、灵敏度高、抗干扰性强等特点。
USA-IL-CIAME followed by high performance liquid chromatography were successfully used for trace detection of flumequine and nalidix acid in chicken and pork.Important parameters affecting extractionefficiency,such as extraction solvent type and volume,anti-sticking agent type and volume,pHandtemperature,were discussed.Linearity of the method was observed over the range 10～300 μg·L~(-1) for flumequine and 5～300μg·L~(-1) for nalidix acid with correlation coefficients up to 0.9995.The sensitivity of the proposed method was found to be excellent with detection limit in range 0.5～0.7μg·L~(-1).The recoveries ranged from 90.4%to 103.2%with relative standard deviations(RSD)from 2.7%to 9.3%.All this resultsindicated that the developed method would be a simple,green and sensitive method.
USA-IL-CIAME followed by high performance liquid chromatography were successfully used for trace detection of flumequine and nalidix acid in chicken and pork.Important parameters affecting extractionefficiency,such as extraction solvent type and volume,anti-sticking agent type and volume,pHandtemperature,were discussed.Linearity of the method was observed over the range 10～300 μg·L~(-1) for flumequine and 5～300μg·L~(-1) for nalidix acid with correlation coefficients up to 0.9995.The sensitivity of the proposed method was found to be excellent with detection limit in range 0.5～0.7μg·L~(-1).The recoveries ranged from 90.4%to 103.2%with relative standard deviations(RSD)from 2.7%to 9.3%.All this resultsindicated that the developed method would be a simple,green and sensitive method.
引文
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[11]Zhao Ru-song,Wang Xia,Sun Jing,et al.Trace Determination of triclosan and Triclocarban in Environmental Water Samples with Ionic Liquid Dispersive Liquid-phase Microextraction Prior to HPLC-ESI MS-MS[J].Anal Bioanal Chem,2010,397(4):1627-1633.
[12]Cheng Ju-fang,Ma Xiao-guo,Wu Yu-guang.silica gel chemically modified with ionic liquid as novel sorbent for solid-phase extraction and preconcentration of lead from beer and tea drink samples followed by flame atomic absorption spectrometric determination[J].Food Anal Method,2014,7:1083-1089.
[2]张兴梅,邓巧巧,李桂芝,等.环境友好型方法快速检测牛奶中的六种喹诺酮残留[J].化学研究与应用,2013,25(9):1303-1307.
[3]Jeong-Heui Choi,Mamun M I R,Abd El-AtyA M,et al.Development of a single-step precipitation cleanup method for the determination of enrofloxacin,ciprofloxacin,and danofloxacin in porcine plasma[J].Food Chem,2011,127:1878-1883.
[4]Qiang Gao,Hao-Bo Zheng,Dan Luo,et al.Facile synthesis of magnetic one-dimensional polyaniline and its application in magnetic solid phase extraction for fluoroquinolones in honeysamples[J].Anal Chim Acta,2012,720:57-62.
[5]Yan-Bo Luo,Qiao Ma,Yu-Qi Feng.Stir rod sorptive extraction with monolithic polymer as coating and its application to the analysis of fluoroquinolones in honey sample[J].J Chromatogr A,2010,1217:3583-3589.
[6]Maria Ramos Payan,Miguel Angel Bello Lopez,Rut Fernandez-Torres,et al.Hollow fiber-based liquid phase microextraction(HF-LPME)as a new approach for the HPLC determination of fluoroquinolones in biological and environmental matrices[J].JPharmaceut Biomed,2011,55:332-341.
[7]Gao Wen-hua,Chen Gao-pan,Chen Yao-wen,et al.Application of single drop liquid-liquid-liquid microextraction for the determination of fluoroquinolones in human urine by capillary electrophoresis[J].J Chromatogr B,2011,879:291-295.
[8]Yu Huan,Tao Yan-fei,Chen Dong-mei,et al.Simultaneous determination of fluoroquinolones in foods of animal origin by a high performance liquid chromatography and a liquid chromatography tandem mass spectrometry with accelerated solvent extraction[J].J Chromatogr B,2012,885-886:150-159.
[9]SunXiao-qi,Luo Hui-min,Dai Sheng.Solvent extraction of rare-earth ions based on functionalized ionic liquids[J].Talanta,2012,90:132-137.
[10]邓凡政,郭东方.离子液体双水相体系萃取分离牛血清白蛋白[J].分析化学,2006,34(10):1451-1453.
[11]Zhao Ru-song,Wang Xia,Sun Jing,et al.Trace Determination of triclosan and Triclocarban in Environmental Water Samples with Ionic Liquid Dispersive Liquid-phase Microextraction Prior to HPLC-ESI MS-MS[J].Anal Bioanal Chem,2010,397(4):1627-1633.
[12]Cheng Ju-fang,Ma Xiao-guo,Wu Yu-guang.silica gel chemically modified with ionic liquid as novel sorbent for solid-phase extraction and preconcentration of lead from beer and tea drink samples followed by flame atomic absorption spectrometric determination[J].Food Anal Method,2014,7:1083-1089.