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Liquid–liquid microextraction of glyphosate, glufosinate and aminomethylphosphonic acid for the analysis of agricultural samples by liquid chromatography
Analytical Methods ( IF 2.7 ) Pub Date : 2020-04-03 , DOI: 10.1039/d0ay00120a
Javier Marín 1, 2, 3, 4, 5 , Natalia Campillo 1, 2, 3, 4, 5 , Manuel Hernández-Córdoba 1, 2, 3, 4, 5 , Isabel Garrido 6, 7, 8, 9 , José Fenoll 6, 7, 8, 9 , Pilar Viñas 1, 2, 3, 4, 5
Affiliation  

A new technique for measurement of glufosinate (GLU), glyphosate (GLY) and its metabolite aminomethylphosphonic acid (AMPA) using liquid chromatography with tandem mass spectrometry with a triple quadrupole (LC-QqQ-MS/MS) is proposed for the analysis of vegetables, agricultural soil and irrigation water. An ion-pair liquid–liquid microextraction (IP-LLME) procedure using 9-fluorenylmethyl chloroformate as the derivatizing reagent, methyl isobutyl ketone as the extraction solvent and hexadecyltrimethylammonium bromide as the ion-pair reagent was performed for preconcentration purposes, because the herbicides are present at very low concentrations. Limits of quantification (LOQs) of 0.5 ng mL−1, 2.5 μg kg−1 and 1.6 μg kg−1 were obtained for water, vegetables and soil, respectively. Repeatability and reproducibility were calculated using the relative standard deviation, and values ranged between 6 and 11%, depending on the analyte. Enrichment factors were 62, 60 and 85 for GLY, GLU and AMPA, respectively.

中文翻译:

草甘膦,草铵膦和氨基甲基膦酸的液-液微萃取用于液相色谱法分析农业样品

提出了一种采用液相色谱-串联质谱联用三重四极杆(LC-QqQ-MS / MS)测定草铵膦(GLU),草甘膦(GLY)及其代谢物氨基甲基膦酸(AMPA)的新技术,农业土壤和灌溉用水。进行离子对液-液微萃取(IP-LLME)程序,以9-芴基甲基氯甲酸酯为衍生剂,甲基异丁基酮为萃取溶剂,十六烷基三甲基溴化铵为离子对试剂,用于预浓缩,因为除草剂是浓度很低。0.5定量限(定量限)纳克毫升-1,2.5微克千克-1和1.6微克千克-1分别用于水,蔬菜和土壤。使用相对标准偏差计算重复性和重现性,其值范围介于6%和11%之间,具体取决于分析物。GLY,GLU和AMPA的富集因子分别为62、60和85。
更新日期:2020-04-24
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