scholarly journals Multi-response optimization of a green solid-phase extraction for the analysis of heterocyclic aromatic amines in environmental samples

2020 ◽  
Vol 12 (11) ◽  
pp. 1504-1513
Author(s):  
Romina Canales ◽  
Leonardo Mariño-Repizo ◽  
Mario Reta ◽  
Soledad Cerutti

A method for the multi-response optimization of a green and efficient solid phase extraction treatment combined with liquid chromatography-tandem mass spectrometry was developed for the quantification of ten heterocyclic aromatic amines in waters.

2020 ◽  
Vol 25 (1) ◽  
Author(s):  
Hiroshi Nomura ◽  
Risa Hamada ◽  
Isao Saito ◽  
Kunihiko Nakane ◽  
Ritsuko Sawa ◽  
...  

Abstract Background Glyphosate and its salt formulations are nonselective herbicides that have been extensively used worldwide, both for residential and agricultural purposes. The possible carcinogenicity and teratogenicity of glyphosate remain to be elucidated. We developed a sensitive and high-throughput analytical method for urinary glyphosate using liquid chromatography-tandem mass spectrometry with the aim of contributing to glyphosate exposure assessment in epidemiological studies. Methods After urine dilution (creatinine matching dilution to 0.05 g creatinine/L), glyphosate was extracted using two types of solid phase extraction columns (SCX and NH2) with automated sample preparation instruments. The eluate was dried and dissolved in the mobile phase, followed by liquid chromatography-tandem mass spectrometry analysis. The optimized method was applied to urine samples obtained from 54 Japanese adults and children. Results The results from the validation study demonstrated good recoveries (91.0-99.6%), within- and between-run precisions (< 15%), low detection limits (0.1 μg/L), and lower limit of quantification (0.3 μg/L). The detection frequency and median concentration of the urinary glyphosate in Japanese subjects were 59% and 0.25 μg/L (0.34 μg/g creatinine). Conclusions Our reliable determination method was successful in measuring urinary glyphosate concentration. Moreover, this is the first biomonitoring report of urinary glyphosate levels in the Japanese general population.


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