当前位置：
X-MOL 学术
›
Anal. Methods
›
论文详情
Our official English website, www.x-mol.net, welcomes your
feedback! (Note: you will need to create a separate account there.)
Quantitative analysis of glyphosate, glufosinate and AMPA in irrigation water by in situ derivatization–dispersive liquid–liquid microextraction combined with UPLC-MS/MS†
Analytical Methods ( IF 2.7 ) Pub Date : 2018-01-03 00:00:00 , DOI: 10.1039/c7ay02722b Edgar Pinto 1, 2, 3, 4, 5 , António Gomes Soares 6, 7, 8 , Isabel M. P. L. V. O. Ferreira 1, 2, 3, 4, 5
Analytical Methods ( IF 2.7 ) Pub Date : 2018-01-03 00:00:00 , DOI: 10.1039/c7ay02722b Edgar Pinto 1, 2, 3, 4, 5 , António Gomes Soares 6, 7, 8 , Isabel M. P. L. V. O. Ferreira 1, 2, 3, 4, 5
Affiliation
|
A novel method was developed for the sensitive, cheap and fast quantitation of glyphosate, glufosinate and aminomethylphosphonic acid (AMPA) in irrigation water by in situ derivatization and dispersive liquid–liquid microextraction (DLLME) combined with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Water samples were filtered with a 0.22 μm nylon filter, pH adjusted to 9 with ammonium bicarbonate and derivatized with fluorenylmethyloxycarbonyl chloride (FMOC-Cl). Afterwards, DLLME was applied to concentrate the compounds of interest, which were then analyzed by UPLC-MS/MS. The best results were obtained when acetone and dichloromethane were used as dispersive and extraction solvents, respectively. Two-level full factorial designs and a central composite design were applied to select the most appropriate derivatization and DLLME conditions. The method performance was evaluated according to the SANTE/11945/2015 guidelines and was linear in the 1.0 to 200 μg L−1 range for glyphosate, glufosinate and AMPA, with r2 ≥ 0.997 and individual residuals <13%. Repeatability (RSDr) and within-laboratory reproducibility (RSDwr) ranged from 2.7 to 9.1% and from 3.4 to 14.3%, respectively, and the trueness between 94.9 and 118.1%. The limits of detection were 0.35, 0.05 and 0.10 μg L−1 for glyphosate, glufosinate and AMPA, respectively and the limit of quantitation was 1.0 μg L−1 for all three compounds. The developed method was successfully applied to the analysis of irrigation water (surface and groundwater). No sign of the three compounds was detected in the groundwater samples but glyphosate was quantified in surface waters.
中文翻译：
原位衍生化-分散液-液微萃取结合UPLC-MS / MS 定量分析灌溉水中的草甘膦，草铵膦和AMPA †
开发了一种新颖，灵敏，便宜而快速的原位定量测定灌溉水中草甘膦，草铵膦和氨基甲基膦酸（AMPA）的方法衍生化和分散液液微萃取（DLLME）结合超高效液相色谱串联质谱法（UPLC-MS / MS）。将水样品用0.22μm尼龙过滤器过滤，用碳酸氢铵将pH调节至9，然后用芴基甲氧基羰基氯（FMOC-Cl）衍生化。之后，使用DLLME浓缩目标化合物，然后通过UPLC-MS / MS分析。当分别使用丙酮和二氯甲烷作为分散溶剂和萃取溶剂时，可获得最佳结果。采用两级全因子设计和中央复合设计来选择最合适的衍生化和DLLME条件。方法性能根据SANTE / 11945/2015指南进行了评估，在1.0至200μgL范围内呈线性关系-1范围为草甘膦，草铵膦和AMPA，用- [R 2 ≥0.997和个人残差<13％。重复性（RSD r）和实验室内可重复性（RSD wr）的范围分别为2.7％至9.1％和3.4％至14.3％，真实性为94.9％至118.1％。检测限为0.35，0.05和0.10微克大号-1草甘膦，草铵膦和AMPA，分别和定量限为1.0微克大号-1的所有三种化合物。所开发的方法已成功地用于灌溉水（地表水和地下水）的分析。在地下水样品中未检测到这三种化合物的迹象，但在地表水中对草甘膦进行了定量。
更新日期：2018-01-03
中文翻译：
原位衍生化-分散液-液微萃取结合UPLC-MS / MS 定量分析灌溉水中的草甘膦，草铵膦和AMPA †
开发了一种新颖，灵敏，便宜而快速的原位定量测定灌溉水中草甘膦，草铵膦和氨基甲基膦酸（AMPA）的方法衍生化和分散液液微萃取（DLLME）结合超高效液相色谱串联质谱法（UPLC-MS / MS）。将水样品用0.22μm尼龙过滤器过滤，用碳酸氢铵将pH调节至9，然后用芴基甲氧基羰基氯（FMOC-Cl）衍生化。之后，使用DLLME浓缩目标化合物，然后通过UPLC-MS / MS分析。当分别使用丙酮和二氯甲烷作为分散溶剂和萃取溶剂时，可获得最佳结果。采用两级全因子设计和中央复合设计来选择最合适的衍生化和DLLME条件。方法性能根据SANTE / 11945/2015指南进行了评估，在1.0至200μgL范围内呈线性关系-1范围为草甘膦，草铵膦和AMPA，用- [R 2 ≥0.997和个人残差<13％。重复性（RSD r）和实验室内可重复性（RSD wr）的范围分别为2.7％至9.1％和3.4％至14.3％，真实性为94.9％至118.1％。检测限为0.35，0.05和0.10微克大号-1草甘膦，草铵膦和AMPA，分别和定量限为1.0微克大号-1的所有三种化合物。所开发的方法已成功地用于灌溉水（地表水和地下水）的分析。在地下水样品中未检测到这三种化合物的迹象，但在地表水中对草甘膦进行了定量。
京公网安备 11010802027423号