柱前衍生-液相色谱法测定土壤中草甘膦和氨甲基膦酸
详细信息 查看官网全文
- 英文论文题名：Determination of Glyphosate and Aminomethyl Phosphonic Acid in Soil Samples by High Performance Liquid Chromatography with Pre-Column Derivatization
- 论文作者：高俊海 ; 宋桂雪 ; 宋薇
- 英文论文作者：Gao Junhai ; Song Guixue ; Song Wei ; Pony Testing International Group
- 年：2016
- 作者机构：谱尼测试集团股份有限公司;
- 论文关键词：土壤样品 ; 草甘膦 ; 氨甲基膦酸 ; 柱前衍生 ; 高效液相色谱-荧光检测
- 英文论文关键词：Soil samples ; glyphosate ; aminomethyl phosphonic acid ; pre-column derivatization ; HPLC-FLD
- 会议召开时间：2016-09-22
- 会议录名称：2016年中国环境与安全监测技术研讨会—第27届MICONEX2016科学仪器惠及民生系列分会场论文集
- 语种：中文
- 分类号：X833;O657.72
- 学会代码：XDKX
- 会议名称：2016年中国环境与安全监测技术研讨会—第27届MICONEX2016科学仪器惠及民生系列分会场
- 会议地点：中国北京
- 主办单位：中国仪器仪表学会
- 学会名称：现代科学仪器编辑部
- 页数：6
- 文件大小：2291k
- 原文格式：D
- 会议级别：全国
摘要
本研究建立了柱前衍生-高效液相色谱-荧光检测法同时测定土壤中草甘膦和氨甲基膦酸(AMPA)残留量的检测方法,并进行了方法参数优化。实验结果表明,按照此方法测定草甘膦和AMPA时峰型尖锐、对称,保留和分离效果好,在2.0μg/L-100μg/L范围内线性关系良好(R2>0.999)。针对土壤样品加标,草甘膦回收率为82.2%-86.8%,RSD%为0.3%-2.5%,AMPA回收率为61.8%-69.1%,RSD%为0.8%-1.2%,说明本方法快捷可靠,精密度高,准确好,满足检测要求。
A method of pre-column derivatization-HPLC-FLD was established for the determination of glyphosate and AMPA in soils by optimizing the experimental conditions. The results showed that both target compounds were well separated in the chromatograms, the peaks are sharp and symmetrical. The standard curves of glyphosate and AMPA are all linearly correlated, respectively,R2> 0.999, with a concentration range of 2.0-100 μg/L. The spiked recoveries of glyphosate in soil samples are in the range of 81.9%-89.3% with the relative standard deviations(RSD) from 0.3 %-2.5%, and the spiked recoveries of AMPA are in the range of 61.2%- 69.4 % with RSD from 0.8%- 1.2%. The method is quick, reliable and has good precision and accuracy.
A method of pre-column derivatization-HPLC-FLD was established for the determination of glyphosate and AMPA in soils by optimizing the experimental conditions. The results showed that both target compounds were well separated in the chromatograms, the peaks are sharp and symmetrical. The standard curves of glyphosate and AMPA are all linearly correlated, respectively,R2> 0.999, with a concentration range of 2.0-100 μg/L. The spiked recoveries of glyphosate in soil samples are in the range of 81.9%-89.3% with the relative standard deviations(RSD) from 0.3 %-2.5%, and the spiked recoveries of AMPA are in the range of 61.2%- 69.4 % with RSD from 0.8%- 1.2%. The method is quick, reliable and has good precision and accuracy.
引文
[1梁诚.草甘膦生产现状与市场分析[J].精细化工原料及中间体,2011,(8):13-15.
[2]卢信,赵炳梓,张佳宝,等.除草剂草甘膦的性质及环境行为综述[J].土壤通报,2005,36(5):785-790.
[3]张伟,王进军,高立明,等.草甘膦在水-土壤系统中的环境行为及研究进展[J].农药,2006,45(10):649-654.
[4]王慧,闫晓红,徐杰,等.我国抗草甘膦基因的发掘现状[J].农业生物技术学报,2014,22(1):109-118.
[5]周垂帆,李莹,张晓勇,等.草甘膦毒性研究进展[J].生态环境学报,2013,22(10):1737-1743.
[6]中华人民共和国卫生部,中国国家标准化管理委员会.GB5749-2006生活饮用水卫生标准[S].北京:中国标准出版社,2006.
[7]Guo ZX,Cai QT,Yang ZG.Ion Chromatography/Inductively coupled plasma mass spectrometry for simultaneous determination of glyphosate,glufosinate,fosamine and ethephon at nanogram levels in water[J].Rapid Commun.Mass Spectrom,2007,21(10):1606-1612.
[8]李祥平,齐剑英,陈永亨,等.离子色谱法测定地表水中的卤乙酸和草甘膦[J].应用化学,2009,26(4):447-450.
[9]张培志,吴军,张培敏,等.土壤中草甘膦的离子色谱法测定[J].分析测试学报,2003,22(4):89-90.
[10]Corbera M,Hidalgo M,SalvadóV,et al.Determination of glyphosate and aminomethylphosphonic acid in natural water using the capillary electrophoresis combined with enrichment step[J].Analytica Chimica Acta,2005,540(1):3-7.
[11]董文庚,陈学诚,朗志敏,等.褪色分光光度法间接测定草甘膦.分析化学,1997,25(10):1210-1212.
[12]Montrap,Jayanta S,Mitras,et al.Micro-scale membrane extraction of glyphosate and aminomethyl phosphonic acid in water followed by high-performance liquid Chromatography and post-column derivatization with fluorescence detector[J].Journal of Chromatography A,2008,1189(1-2):483-492.
[13]Qian K,Tang T,Shi TY,et al.Residue determination of glyphosate in environmental water samples with high-performance liquid Chromatography and UVdetection after derivatization with 4-chloro-3,5-dinitrobenzotrifluoride[J].Analytica Chimica Acta,2009,635(2):222-226.
[14]张蓓蓓,张立志,章勇.水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究[J].环境监控与预警,2015,7(2):13-19.
[15]胡继业,赵殿英,宁君,等.气相色谱-氮磷检测器测定草甘膦在土壤和苹果中的残留量[J].农药学学报,2007,9(3):285-290.
[16]马为民,牛森,李东运,等.气相色谱法测定几种蔬菜水果中草甘膦残留[J].农药,2006,45(4):261-262.
[17]程雪梅,周敏.气相色谱-质谱法测定香蕉和灌溉水中的草甘膦及其代谢物的残留量[J].色谱,2004,22(3):288.
[18]Hao CY,Morse D,Motta F,et al.Direct aqueous determination of glyphosate and related compounds by liquid Chromatography/tandem mass spectrometry using reversed-phase and weak anion-exchange mixed-mode column[J].Journal of Chromatography A,2011,1218(33):5638-5643.
[19]Sanchis J,Kantiani L,Llorca M,et al.Determination of glyphosate in groundwater samples using an ultrasensitive immunoassay and confirmation by on-line solidphase extraction followed by liquid Chromatography coupled to tandem mass spectrometry[J].Anal Bioanal Chem,2012,402(7):2335-2345.
[20]Hanke I,Singer H,Hollender J,et al.Ultratrace-level determination of glyphosate,aminomethylphosphonic acid and glufosinate in natural waters by solidphase extraction followed by liquid Chromatographytandem mass spectrometry:performance tuning of derivatization,enrichment and detection[J].Anal Bioanal Chem,2008,391(6):2265-2276.
[21]郑和辉,张静,李洁,等.超高效液相色谱串联质谱法直接进样测定水中的草甘膦和呋喃丹[J].分析试验室,2008,27(12):68-70.
[22]刘拉平,武瑜,王玉堂,等.柱前衍生高效液相色谱-串联质谱法测定土壤中草甘膦及其主要代谢物氨甲基膦酸[J].农药学学报,2015,17(4):439-446.
[23]成婧,王美玲,龚强,等.液相色谱-串联质谱法检测植物源食品中草甘膦及其代谢物的残留量.食品安全质量检测学报,2016,7(1):138-144.
[24]诸力,陈红平,周苏娟,等.超高效液相色谱-串联质谱法测定不同茶叶中草甘膦、氨甲基膦酸及草铵膦的残留[J].分析化学研究报告,2015,43(2):271-276.
[25]Roy D N,陆贻通.土壤中草甘膦及其代谢产物残留测定方法的改进[J].农药译丛,1990,12(3):47-49.
[26]司友斌,桑忠营,程凤侠.对甲基苯磺酰氯衍生化液相色谱法测定土壤中草甘膦[J].安徽农业大学学报,2009,36(1):136-139.
[27]张培志,吴军,张培敏,等.土壤中草甘膦的离子色谱法测定[J].分析测试学报,2003,22(4):89-90.
[28]汪立高,杨仁斌,魏凤.土壤中残留草甘膦检测方法及其消解动态研究[J].湖南农业科学,2011(23):85-88.
[2]卢信,赵炳梓,张佳宝,等.除草剂草甘膦的性质及环境行为综述[J].土壤通报,2005,36(5):785-790.
[3]张伟,王进军,高立明,等.草甘膦在水-土壤系统中的环境行为及研究进展[J].农药,2006,45(10):649-654.
[4]王慧,闫晓红,徐杰,等.我国抗草甘膦基因的发掘现状[J].农业生物技术学报,2014,22(1):109-118.
[5]周垂帆,李莹,张晓勇,等.草甘膦毒性研究进展[J].生态环境学报,2013,22(10):1737-1743.
[6]中华人民共和国卫生部,中国国家标准化管理委员会.GB5749-2006生活饮用水卫生标准[S].北京:中国标准出版社,2006.
[7]Guo ZX,Cai QT,Yang ZG.Ion Chromatography/Inductively coupled plasma mass spectrometry for simultaneous determination of glyphosate,glufosinate,fosamine and ethephon at nanogram levels in water[J].Rapid Commun.Mass Spectrom,2007,21(10):1606-1612.
[8]李祥平,齐剑英,陈永亨,等.离子色谱法测定地表水中的卤乙酸和草甘膦[J].应用化学,2009,26(4):447-450.
[9]张培志,吴军,张培敏,等.土壤中草甘膦的离子色谱法测定[J].分析测试学报,2003,22(4):89-90.
[10]Corbera M,Hidalgo M,SalvadóV,et al.Determination of glyphosate and aminomethylphosphonic acid in natural water using the capillary electrophoresis combined with enrichment step[J].Analytica Chimica Acta,2005,540(1):3-7.
[11]董文庚,陈学诚,朗志敏,等.褪色分光光度法间接测定草甘膦.分析化学,1997,25(10):1210-1212.
[12]Montrap,Jayanta S,Mitras,et al.Micro-scale membrane extraction of glyphosate and aminomethyl phosphonic acid in water followed by high-performance liquid Chromatography and post-column derivatization with fluorescence detector[J].Journal of Chromatography A,2008,1189(1-2):483-492.
[13]Qian K,Tang T,Shi TY,et al.Residue determination of glyphosate in environmental water samples with high-performance liquid Chromatography and UVdetection after derivatization with 4-chloro-3,5-dinitrobenzotrifluoride[J].Analytica Chimica Acta,2009,635(2):222-226.
[14]张蓓蓓,张立志,章勇.水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究[J].环境监控与预警,2015,7(2):13-19.
[15]胡继业,赵殿英,宁君,等.气相色谱-氮磷检测器测定草甘膦在土壤和苹果中的残留量[J].农药学学报,2007,9(3):285-290.
[16]马为民,牛森,李东运,等.气相色谱法测定几种蔬菜水果中草甘膦残留[J].农药,2006,45(4):261-262.
[17]程雪梅,周敏.气相色谱-质谱法测定香蕉和灌溉水中的草甘膦及其代谢物的残留量[J].色谱,2004,22(3):288.
[18]Hao CY,Morse D,Motta F,et al.Direct aqueous determination of glyphosate and related compounds by liquid Chromatography/tandem mass spectrometry using reversed-phase and weak anion-exchange mixed-mode column[J].Journal of Chromatography A,2011,1218(33):5638-5643.
[19]Sanchis J,Kantiani L,Llorca M,et al.Determination of glyphosate in groundwater samples using an ultrasensitive immunoassay and confirmation by on-line solidphase extraction followed by liquid Chromatography coupled to tandem mass spectrometry[J].Anal Bioanal Chem,2012,402(7):2335-2345.
[20]Hanke I,Singer H,Hollender J,et al.Ultratrace-level determination of glyphosate,aminomethylphosphonic acid and glufosinate in natural waters by solidphase extraction followed by liquid Chromatographytandem mass spectrometry:performance tuning of derivatization,enrichment and detection[J].Anal Bioanal Chem,2008,391(6):2265-2276.
[21]郑和辉,张静,李洁,等.超高效液相色谱串联质谱法直接进样测定水中的草甘膦和呋喃丹[J].分析试验室,2008,27(12):68-70.
[22]刘拉平,武瑜,王玉堂,等.柱前衍生高效液相色谱-串联质谱法测定土壤中草甘膦及其主要代谢物氨甲基膦酸[J].农药学学报,2015,17(4):439-446.
[23]成婧,王美玲,龚强,等.液相色谱-串联质谱法检测植物源食品中草甘膦及其代谢物的残留量.食品安全质量检测学报,2016,7(1):138-144.
[24]诸力,陈红平,周苏娟,等.超高效液相色谱-串联质谱法测定不同茶叶中草甘膦、氨甲基膦酸及草铵膦的残留[J].分析化学研究报告,2015,43(2):271-276.
[25]Roy D N,陆贻通.土壤中草甘膦及其代谢产物残留测定方法的改进[J].农药译丛,1990,12(3):47-49.
[26]司友斌,桑忠营,程凤侠.对甲基苯磺酰氯衍生化液相色谱法测定土壤中草甘膦[J].安徽农业大学学报,2009,36(1):136-139.
[27]张培志,吴军,张培敏,等.土壤中草甘膦的离子色谱法测定[J].分析测试学报,2003,22(4):89-90.
[28]汪立高,杨仁斌,魏凤.土壤中残留草甘膦检测方法及其消解动态研究[J].湖南农业科学,2011(23):85-88.