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目的为了缩短样品的检测时间,同时对国标方法中涉及的参数展开系统的优化,以提高水样中痕量草甘膦的检测灵敏度。方法以水、磷酸、硫酸为流动相,经等度洗脱后,进行柱后衍生,最后在激发波长为330 nm、发射波长为460 nm条件下,进行荧光检测。结果与液相色谱相比,超高效液相色谱使分离时间从8 min缩短至4 min;与国标方法相比,本方法的检出限降低至0.19 ng/ml,灵敏度提高了130倍;方法的线性相关系数为0.9998,回收率为96.0%~100.1%,RSD为0.3%~1.6%。结论超高效液相色谱柱后衍生法分析时间短、灵敏度高,完全能满足水样中草甘膦分析检测的需求。
Objective In order to shorten the detection time of the sample, meanwhile, the parameters involved in the national standard method were systematically optimized to improve the detection sensitivity of trace glyphosate in water sample. Methods After water, phosphoric acid and sulfuric acid were used as mobile phases, the isocratic elution was carried out and the column derivatization was carried out. Finally, the fluorescence was detected under the conditions of an excitation wavelength of 330 nm and an emission wavelength of 460 nm. Results Compared with liquid chromatography, the separation time was shortened from 8 min to 4 min by ultra performance liquid chromatography. Compared with the national standard method, the detection limit of this method was reduced to 0.19 ng / ml and the sensitivity was improved by 130 times. Methods The linear correlation coefficient was 0.9998, the recovery was 96.0% ~ 100.1%, RSD was 0.3% ~ 1.6%. Conclusion The method of post-column derivatization with ultra-performance liquid chromatography has short time and high sensitivity, which can fully meet the needs of glyphosate analysis and detection in water sample.