超高效液相色谱串联质谱法测定咖啡豆中草甘膦、氨甲基膦酸和草铵膦残留量

Determination of glyphosate, aminomethyl phosphoric acid and glufosinate residue in coffee bean by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱法  草甘膦  氨甲基膦酸  草铵膦  咖啡豆

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  glyphosate  aminomethyl phosphoric acid  glufosinate  coffee bean

中文摘要:

      目的 建立超高效液相色谱串联质谱法(ultra performance liquid chromat-ography/tandem mass spectrometry, UPLC-MS/MS)定量测定咖啡豆中草甘膦、氨甲基膦酸和草铵膦残留量。方法 通过水提取样品, C18固相萃取小柱进行净化, FMOC-Cl溶液衍生, 后采用超高效液相色谱串联质谱测定。结果 草甘膦、氨甲基膦酸和草铵膦在2~100 ng/mL范围内线性良好(r2≥0.999), 方法的定量限为0.05 mg/kg。在添加水平为 0.05 mg/kg和0.5 mg/kg时, 回收率为99.6%~107.6%, 相对标准偏差低于4.52%。结论 该方法准确、稳定、灵敏, 能够满足咖啡豆中草甘膦、氨甲基膦酸和草铵膦检测与确证的需要。

英文摘要:

      Objective To establish a quantitative method for the determination of glyphosate, aminomethylphosphonic acid and glufosinate residues in coffee beans by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted by water, purified by C18 solid phase extraction column, derivatized by FMOC-Cl solution, and then determined by UPLC-MS/MS. Results Glyphosate, aminomethyl phosphonic acid and glufosinate had good linearity in the range of 2–100 ng/mL (r2≥0.999), and the quantitative limit of the method was 0.05 mg/kg. The recoveries were 99.6%–107.6% and the relative standard deviation was less than 4.52% at 0.05 mg/kg and 0.5 mg/kg. Conclusion This method is accurate, stable and sensitive, and can meet the needs of the detection and confirmation of glyphosate, aminomethyl phosphoric acid and glyphosate in coffee beans.