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目的建立快速、准确的蔬菜中草甘膦的柱前衍生-固相萃取-高效液相色谱荧光测定方法。方法蔬菜提取液样经衍生后经固相萃取,过C_(18)色谱柱,以甲醇-水(70:30,V:V)为流动相,流速1.0 mL/min,柱温为35℃,荧光检测激发波长为265 nm,发射波长为3 15 nm。结果草甘膦的加标回收率在89.2%~99.2%范围,其相对标准偏差均<5.0%,在0.5~20.0 ng/mL范围呈现良好的线性,其回归系数>0.999,最低定量检出限(LOQ)为0.02 mg/kg。结论本方法回收率高,净化效果好,杂质干扰少,可满足蔬菜中痕量草甘膦的残留检测要求。
OBJECTIVE To establish a rapid and accurate method for determination of glyphosate in vegetables by pre-column derivatization-solid phase extraction-high performance liquid chromatography (HPLC). Methods The samples of vegetable extracts were subjected to solid phase extraction and column chromatography on a C 18 column with methanol-water (70:30, V: V) as mobile phase at a flow rate of 1.0 mL / min. The column temperature was 35 ℃, Fluorescence detection excitation wavelength of 265 nm, emission wavelength of 3 15 nm. Results The spiked recoveries of glyphosate ranged from 89.2% to 99.2%. The relative standard deviations (RSDs) were all less than 5.0%. The linearity ranged from 0.5 to 20.0 ng / mL with the regression coefficient> 0.999. The lowest limit of quantification (LOQ) of 0.02 mg / kg. Conclusion The method has high recovery rate, good purification effect and less impurity interference, which can meet the residue detection requirements of trace glyphosate in vegetables.