分散液—液微萃取—液相色谱法测定水中常见抗生素的研究
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摘要
目的建立分散液—液微萃取—液相色谱法测定水中9种抗生素。方法水样经萃取浓缩后液相色谱法测定。结果方法在(5.00～50.0)μg/L范围的相关系数为0.998 1～0.999 4;方法的检出限(0.43～1.57)μg/L、定量限(1.33～5.33)μg/L;回收率66.4%～94.0%,相对标准偏差为1.5%～6.5%。结论该方法操作简便、准确,适用于水样中痕量抗生素的测定。
Objectives A method was established for the detection of nine antibiotics in water samples by dispersive liquid-liquid microextraction coupled with liquid chromatography(DLLME-LC). Methods After concentration, extracts were analyzed by LC. Results The calibration curves ranged from 5.00 μg/L to 50.0 μg/L with the correlation coefficients of 0.998 1～0.999 4 for antibiotics. The Limits of Detections(LODs) and limits of quantification(LOQs) were in the range of(0.43～1.57) μg/L and(1.33～5.33) μg/L, respectively. The recoveries for antibiotics were in the range of 66.4%～94.0% with the relative standard deviations(n=5) of 1.5%～6.5%. Conclusions The method was simple, sensitive and accurate, which could be applied to the detection of trace antibiotics in water samples.
Objectives A method was established for the detection of nine antibiotics in water samples by dispersive liquid-liquid microextraction coupled with liquid chromatography(DLLME-LC). Methods After concentration, extracts were analyzed by LC. Results The calibration curves ranged from 5.00 μg/L to 50.0 μg/L with the correlation coefficients of 0.998 1～0.999 4 for antibiotics. The Limits of Detections(LODs) and limits of quantification(LOQs) were in the range of(0.43～1.57) μg/L and(1.33～5.33) μg/L, respectively. The recoveries for antibiotics were in the range of 66.4%～94.0% with the relative standard deviations(n=5) of 1.5%～6.5%. Conclusions The method was simple, sensitive and accurate, which could be applied to the detection of trace antibiotics in water samples.
引文
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[7] Phiroonsoontorn N,Sansuk S,Santaladchaiyakit Y,et al.The use of dissolvable layered double hydroxide components in an in situ solid-phase extraction for chromatographic determination of tetracyclines in water and milk samples[J].J Chromatogr A,2017,1519:38-44.
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[9] 王栋纬,宋燕西,冶晓凡,等.氧化石墨烯对磺胺甲恶唑和磺胺甲基嘧啶的吸附性能研究[J].分析化学,2018,46(2):211-216.(In English:Wang DW,Song YX,Ye XF,et al.Study on adsorption of two sulfonamide antibiotics by graphene oxide[J].Chin J Anal Chem,2018,46(2):211-216.)
[10] Bayen S,Yi XZ,Segovia E,et al.Analysis of selected antibiotics in surface freshwater and seawater using direct injection in liquid chromatography electrospray ionization tandem mass spectrometry[J].J Chromatogr A,2014,1338:38-43.
[11] 余胜兵,郑惠东,鲁琳,等.超高效液相色谱—串联质谱同时测定饮用水中60种抗生素[J].环境卫生学杂志,2018,8(3):261-269.(In English:Yu SB,Zheng HD,Lu L,et al.Simultaneous determination of 60 kinds of antibiotics in drinking water samples by ultra-performance liquid chromatography-tandem mass spectrometry[J].J Environ Hyg,2018,8(3):261-269.)
[12] Richardson SD,Ternes TA.Water analysis:emerging contaminants and current issues[J].Anal Chem,2014,86(6):2813-2848.
[13] Andrés-Costa MJ,Andreu V,Picó Y.Analysis of psychoactive substances in water by information dependent acquisition on a hybrid quadrupole time-of-flight mass spectrometer[J].J Chromatogr A,2016,1461:98-106.
[14] 李晓晶,于鸿,甘平胜.超高效液相色谱—串联质谱法测定土壤中多种兽用抗生素残留[J].环境卫生学杂志,2016,6(4):296-299.(In English:Li XJ,Yu H,Gan PS.Determination of antibiotic residues in soil by UPLC-MS/MS[J].J Environ Hyg,2016,6(4):296-299.)
[15] Herrera-Herrera AV,Hernández-Borges J,Borges-Miquel TM,et al.Dispersive liquid-liquid microextraction combined with ultra-high performance liquid chromatography for the simultaneous determination of 25 sulfonamide and quinolone antibiotics in water samples[J].J Pharm Biomed Anal,2013,75:130-137.
[16] Vázquez MMP,Vázquez PP,Galera MM,et al.Determination of eight fluoroquinolones in groundwater samples with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction prior to high-performance liquid chromatography and fluorescence detection[J].Anal Chim Acta,2012,748:20-27.
[2] 郑惠东.水环境中抗生素来源及对健康的影响[J].环境卫生学杂志,2018,8(1):73-77.(In English:Zheng HD.The source of antibiotics in aquatic environment and its impact on human health[J].J Environ Hyg,2018,8(1):73-77.)
[3] Kolpin DW,Furlong ET,Meyer MT,et al.Pharmaceuticals,hormones,and other organic wastewater contaminants in U.S.streams,1999-2000:a national reconnaissance[J].Environ Sci Technol,2002,36(6):1202-1211.
[4] Valcárcel Y,Alonso SG,Rodríguez-Gil JL,et al.Detection of pharmaceutically active compounds in the rivers and tap water of the Madrid region (Spain) and potential ecotoxicological risk[J].Chemosphere,2011,84(10):1336-1348.
[5] 王丹,隋倩,赵文涛,等.中国地表水环境中药物和个人护理品的研究进展[J].科学通报,2014,59(9):743-751.(In English:Wang D,Sui Q,Zhao WT,et al.Pharmaceutical and personal care products in the surface water of China:a review[J].Chin Sci Bull,2014,59(9):743-751.)
[6] Gatidou G,Thomaidis NS,Stasinakis AS,et al.Simultaneous determination of the endocrine disrupting compounds nonylphenol,nonylphenol ethoxylates,triclosan and bisphenol A in wastewater and sewage sludge by gas chromatography-mass spectrometry[J].J Chromatogr A,2007,1138(1-2):32-41.
[7] Phiroonsoontorn N,Sansuk S,Santaladchaiyakit Y,et al.The use of dissolvable layered double hydroxide components in an in situ solid-phase extraction for chromatographic determination of tetracyclines in water and milk samples[J].J Chromatogr A,2017,1519:38-44.
[8] Xu X,Su R,Zhao X,et al.Ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction and derivatization of sulfonamides in river water,honey,milk,and animal plasma[J].Anal Chim Acta,2011,707(1-2):92-99.
[9] 王栋纬,宋燕西,冶晓凡,等.氧化石墨烯对磺胺甲恶唑和磺胺甲基嘧啶的吸附性能研究[J].分析化学,2018,46(2):211-216.(In English:Wang DW,Song YX,Ye XF,et al.Study on adsorption of two sulfonamide antibiotics by graphene oxide[J].Chin J Anal Chem,2018,46(2):211-216.)
[10] Bayen S,Yi XZ,Segovia E,et al.Analysis of selected antibiotics in surface freshwater and seawater using direct injection in liquid chromatography electrospray ionization tandem mass spectrometry[J].J Chromatogr A,2014,1338:38-43.
[11] 余胜兵,郑惠东,鲁琳,等.超高效液相色谱—串联质谱同时测定饮用水中60种抗生素[J].环境卫生学杂志,2018,8(3):261-269.(In English:Yu SB,Zheng HD,Lu L,et al.Simultaneous determination of 60 kinds of antibiotics in drinking water samples by ultra-performance liquid chromatography-tandem mass spectrometry[J].J Environ Hyg,2018,8(3):261-269.)
[12] Richardson SD,Ternes TA.Water analysis:emerging contaminants and current issues[J].Anal Chem,2014,86(6):2813-2848.
[13] Andrés-Costa MJ,Andreu V,Picó Y.Analysis of psychoactive substances in water by information dependent acquisition on a hybrid quadrupole time-of-flight mass spectrometer[J].J Chromatogr A,2016,1461:98-106.
[14] 李晓晶,于鸿,甘平胜.超高效液相色谱—串联质谱法测定土壤中多种兽用抗生素残留[J].环境卫生学杂志,2016,6(4):296-299.(In English:Li XJ,Yu H,Gan PS.Determination of antibiotic residues in soil by UPLC-MS/MS[J].J Environ Hyg,2016,6(4):296-299.)
[15] Herrera-Herrera AV,Hernández-Borges J,Borges-Miquel TM,et al.Dispersive liquid-liquid microextraction combined with ultra-high performance liquid chromatography for the simultaneous determination of 25 sulfonamide and quinolone antibiotics in water samples[J].J Pharm Biomed Anal,2013,75:130-137.
[16] Vázquez MMP,Vázquez PP,Galera MM,et al.Determination of eight fluoroquinolones in groundwater samples with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction prior to high-performance liquid chromatography and fluorescence detection[J].Anal Chim Acta,2012,748:20-27.