柱前衍生高效液相色谱法测定饮用水中草甘膦、草铵膦和氨甲基膦酸

发布时间：2018-08-19 19:10

【摘要】：目的建立柱前衍生-固相萃取-液相色谱-荧光法测定饮用水中草甘膦、草铵膦和氨甲基膦酸的方法。方法样品经衍生和固相萃取后,采用Waters Atlantis T3(4.6 mm×250 mm,5μm)色谱柱分离,流动相为甲醇-0.02 mol/L乙酸铵水溶液(50∶50,V/V),流速1.0 ml/min,荧光检测激发波长为266 nm,发射波长为315 nm,进样体积为10μl。结果 3种目标物质在0.01~1.0 mg/L范围内线性良好,线性相关系数(r)均在0.9994~0.9998之间。通过对自来水样进行3个加标水平的添加回收试验(n=6),草甘膦、草铵膦和氨甲基膦酸的平均回收率分别为84.4%~92.0%、86.5%~93.8%和87.8%~96.8%,相对标准偏差(RSD)分别为1.12%~4.22%、1.05%~4.04%和1.08%~3.95%,方法的检出限分别为0.0021、0.0025和0.0032mg/L。结论该方法准确灵敏,适用于饮用水中草甘膦、草铵膦和氨甲基膦酸3种物质的同时分析。
[Abstract]:Objective to establish a method for the determination of glyphosate, glyphosate and aminomethylphosphonic acid in drinking water by pre-column derivatization-solid phase extraction-liquid chromatography-fluorescence method. Methods the samples were separated by Waters Atlantis T3 (4.6mm 脳 250mm ~ 5 渭 m) column after derivatization and solid-phase extraction. The mobile phase was methanol-0.02 mol/L ammonium acetate solution (50: 50 V / V), the flow rate was 1.0 ml / min, the fluorescence detection excitation wavelength was 266nm, the emission wavelength was 315nm, and the sample volume was 10 渭 l. Results the linear correlation coefficient (r) of the three target substances was between 0.9994 and 0.9998 in the range of 0.01 ~ 1.0 mg/L. The average recoveries of glyphosate, ammonium oxalate and aminomethylphosphonic acid were 84.42.0.92% and 86.5% and 87.8% respectively. The relative standard deviation (RSD) was 1.124.221.051.04% and 1.08g / 3.955.The detection limits of the method were 0.0021mg0.0025 and 32mg / L, respectively. The average recoveries of glyphosate, ammonium oxalate and aminomethylphosphonic acid were 0.0021.0025 and 32mgL / L, respectively, and the relative standard deviations (RSD) were 1.124.221.051.04% and 1.080.95%, respectively. Conclusion the method is accurate and sensitive and suitable for simultaneous analysis of glyphosate, glyphosate and aminomethylphosphonic acid in drinking water.
【作者单位】：江苏省泰州市疾病预防控制中心;
【分类号】：R123.1;O657.72

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