Determination of Glyphosate and Aminomethylphosphonic Acid in Drinking Water by SPE-HPLC Combined with Pre-Column Derivatization
摘 要
提出了柱前衍生-固相萃取-高效液相色谱法测定饮用水中草甘膦和氨甲基膦酸。水样经9-芴基甲基三氯甲烷衍生和C18固相萃取小柱净化后,洗脱液采用Waters Atlantis T3色谱柱分离,流动相为甲醇-0.02 mol·L-1乙酸铵溶液(60+40),荧光检测器激发波长为266 nm,发射波长为315 nm。草甘膦和氨甲基膦酸的质量浓度在5.00~500 μg·L-1范围内与其峰面积呈线性关系,检出限均为0.002 μg·L-1。对水样进行加标回收试验,草甘膦和氨甲基膦酸的回收率分别在84.4%~92.0%和87.8%~96.8%之间,相对标准偏差(n=6)分别在1.2%~4.3%和1.1%~4.0%之间。该方法适用于水厂出水水样中草甘膦和氨甲基膦酸的同时测定。
Abstract
A method of SPE-HPLC coupled with pre-column derivatization was proposed for the determination of glyphosate and aminomethylphosphonic acid in drinking water. Water sample was derived with FMOC-Cl and purified by C18 solid phase extraction column. The derivatives were separated on an Atlantis T3 column with a mixture of methanol and 0.02 mol·L-1 of ammonium acetate (60+40) as mobile phase. The wavelengths of fluorescence excitation and emission used were 266 nm and 315 nm respectively. The linear relationship between the peak area and the mass concentration of glyphosate and aminomethylphosphonic acid were in the range of 5.00-500 μg·L-1, with detection limits (3S/N) of 0.002 μg·L-1. The recovery rates measured by adding standard samples to water sample were in the range of 84.4%-92.0% and 87.8%-96.8% for glyphosate and aminomethylphosphonic acid respectively, with RSD (n=5) in the range of 1.2%-4.3% and 1.1%-4.0% respectively. The method was used for simultaneous determination of glyphosate and aminomethylphosphonic acid in water samples of water supply plants.
中图分类号 O652.63
所属栏目 工作简报
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收稿日期 2014/3/28
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备注杨华梅(1978-),女,江苏姜堰人,高级工程师,硕士,主要从事食品安全检测工作。
引用该论文: YANG Hua-mei,HANG Li. Determination of Glyphosate and Aminomethylphosphonic Acid in Drinking Water by SPE-HPLC Combined with Pre-Column Derivatization[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(4): 474~477
杨华梅,杭莉. 柱前衍生-固相萃取-高效液相色谱法测定饮用水中草甘膦和氨甲基膦酸[J]. 理化检验-化学分册, 2015, 51(4): 474~477
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参考文献
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【4】GB 5749-2006生活饮用水卫生标准[S].
【5】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):288-288.
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【12】曹丽伟,梁丝柳,谭小芳,等.毛细管电泳-激光诱导荧光法测定草甘膦、草胺膦及氨甲基膦酸[J].色谱, 2012,12(3):1295-1300.
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【14】SN/T 1923-2007进出口食品中草甘膦残留量的检测方法 液相色谱-质谱/质谱法[S].
【15】周爽,徐敦明,林立毅,等.反相色谱-串联质谱法直接测定植物源性食品中草甘膦及其代谢物残留[J].分析测试学报, 2013,32(2):199-204.
【16】江燕,曹赵云,贾瑞琳,等.亲水作用色谱-串联质谱法测定稻米中的草甘膦和氨甲基膦酸残留量[J].色谱, 2012,30(1):39-44.
【17】李波,邓晓军,郭德华,等.高效液相色谱-串联质谱法检测食品中的草甘膦及其主要代谢物氨甲基膦酸残留[J].色谱, 2007,25(4):486-490.
【18】ZAVITSANOS P, MENG Chin-kai.液相色谱/电喷雾-质谱联用检测草甘膦和氨甲基膦酸[J].环境化学, 2003,22(3):303-306.
【19】GRANBY K, JOHANNESEN S, VAHL M. Analysis of glyphosate residues in cereals using liquid chromatography mass spectrometry[J]. Food Addit Contam, 2003,20(8):692-698.
【20】VREEKEN R J, SPEKSNIJDER P, BOBELDIJK-PASTOROVAL, et al. Selective analysis of the herbicides glyphosate and aminomethylphosphonic acid in water by on-line solid-phase extraction high performance liquid chromatography electrospray ionization mass spectrometry[J]. Journal of Chromatography A, 1998,794(1/2):187-199.
【2】李建平,渠志华,马永民,等.饮用水中草甘膦残留量的柱前衍生-高效液相色谱测定法[J].环境与健康杂志, 2012,29(10):73-74.
【3】RUBIN J L, GAINES C G, JENSEN R A. Enzymological basis for herbicidal action of glyphosate[J]. Plant Physiolog, 1982,70:833-839.
【4】GB 5749-2006生活饮用水卫生标准[S].
【5】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):288-288.
【6】GB/T 5750.9-2006生活饮用水标准检验方法[S].
【7】汪琳,曾锦明,韩燕飞,等.直接进样高效液相色谱-柱后衍生法检测水中草甘膦和氨甲基膦酸[J].现代科学仪器, 2010,12(6):99-101.
【8】HOGENDOORN E A, OSSENDRIJVER F M DIJKMAN E, et al. Rapid determination of glyphosate in cereal samples by means of pre-colum derivatisation with 9-fluorenylmethyl chloroformate and coupled colum liquid chromatography with fluorescence detection[J]. Journal of Chromatography A, 1999,833(1):67-73.
【9】FELIX H, CARMEN H, JUAN V S. Determination of glyphosate residues in plants by precolumn derivatization and coupled-column liquid chromatography with fluorescence detection[J]. Journal of Aoac International, 2000,83(3):728-734.
【10】NEDELKOSKA T V, LOW G K C. High-performanic liquid chromatographic determination of glyphosate in water and plant material after pre-column derivatisation with 9-gluorenylmthyl chloroformate[J]. Analytica Chimica Acta, 2004,511(1):145-153.
【11】SANCHO J V, HERNANDES F, LOPEZ F J, et al. Rapid determination of glufosinate, glyphosate and aminomethylphosphonic acid in environmental water samples using precolumn fluorogenic labling and coupled-column liquid chromatography[J]. Journal of Chromatography A, 1996,737(1):75-83.
【12】曹丽伟,梁丝柳,谭小芳,等.毛细管电泳-激光诱导荧光法测定草甘膦、草胺膦及氨甲基膦酸[J].色谱, 2012,12(3):1295-1300.
【13】SARAH Y C, CHIA-HUNG L. Analysis of glyphosate, glufosinate and aminomethylphosphonic acid by capillary electrophoresis with indirect fluorescence detection[J]. Journal of Chromatoqraphy A, 2002,959(1/2):309-315.
【14】SN/T 1923-2007进出口食品中草甘膦残留量的检测方法 液相色谱-质谱/质谱法[S].
【15】周爽,徐敦明,林立毅,等.反相色谱-串联质谱法直接测定植物源性食品中草甘膦及其代谢物残留[J].分析测试学报, 2013,32(2):199-204.
【16】江燕,曹赵云,贾瑞琳,等.亲水作用色谱-串联质谱法测定稻米中的草甘膦和氨甲基膦酸残留量[J].色谱, 2012,30(1):39-44.
【17】李波,邓晓军,郭德华,等.高效液相色谱-串联质谱法检测食品中的草甘膦及其主要代谢物氨甲基膦酸残留[J].色谱, 2007,25(4):486-490.
【18】ZAVITSANOS P, MENG Chin-kai.液相色谱/电喷雾-质谱联用检测草甘膦和氨甲基膦酸[J].环境化学, 2003,22(3):303-306.
【19】GRANBY K, JOHANNESEN S, VAHL M. Analysis of glyphosate residues in cereals using liquid chromatography mass spectrometry[J]. Food Addit Contam, 2003,20(8):692-698.
【20】VREEKEN R J, SPEKSNIJDER P, BOBELDIJK-PASTOROVAL, et al. Selective analysis of the herbicides glyphosate and aminomethylphosphonic acid in water by on-line solid-phase extraction high performance liquid chromatography electrospray ionization mass spectrometry[J]. Journal of Chromatography A, 1998,794(1/2):187-199.
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