Liquid–liquid microextraction of glyphosate, glufosinate and aminomethylphosphonic acid for the analysis of agricultural samples by liquid chromatography,Analytical Methods

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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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