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Determination of glyphosate and glufosinate in human serum by monospin TiO extraction and liquid chromatography–tandem mass spectrometry

Saito Takeshi, Namera Akira, Tsuji Tomoatsu, Noguchi Wataru, Inokuchi Sadaki

Acta Chromatographica

2020

Vol. 32, no. 1

10--15

We developed and validated an assay for determination of glyphosate (GLYP) and glufosinate (GLUF) in human serum. Serum samples were extracted by using a MonoSpin® TiO column and analyzed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). MonoSpin® TiO tends to specifically bind to phosphate groups. The assay was linear over a concentration range of 1–250 μg/mL. The recoveries for the 2 compounds were 1.6%–2.3%. The intra- and inter-day variations were <15%. Precision and accuracy were 5.6%–12.7% and 97.0%–103.9%, respectively. The validated method was applied to quantify the GLYP and GLUF content in the serum of GLYP and GLUF-poisoned patients. In conclusion, the method was successfully applied for accurate determination of GLYP and GLUF in serum obtained from patients with GLYP and GLUF poisoning.

Hydrophilic-interaction liquid chromatography (HILIC) with dad and mass spectroscopic detection for direct analysis of glyphosate and glufosinate residues and for product quality control

Li X., Xu J., Jiang Y., Chen L, Xu Y., Pan C.

Acta Chromatographica

2009

Vol. 21, no. 4

559--576

High-performance liquid chromatography with a hydrophilic-interaction liquid chromatographic (HILIC) column has been successfully used to retain and separate the polar phosphonic herbicides glyphosate and glufosinate. Online electrospray tandem ion-trap mass spectrometric and DAD detection were used. The effects on the separation of mobile phase acetonitrile content, buffer concentration, and flow rate, and of column temperature, were investigated. With UV-visible detection at 195 nm, LOQ were <850 mg kg -1, showing the method is suitable for product quality control of these herbicides alone or in combination. Tandem mass spectrometric conditions were optimized for ion-trap detection. Quantification was by use of selected reaction monitoring transitions m / z 168 → 150 in negative-ion mode for glyphosate and m / z 182 → 136 in positive-ion mode for glufosinate. Limits of detection (LOD; S / N > 3) were 0.20 and 0.16 ng for glyphosate and glufosinate, respectively, and the respective limits of quantification (LOQ; S / N = 10) were 0.02 and 0.05 mg kg -1 . Sample derivatization was not necessary to achieve low detection limits in residue analysis in this study. Recovery from watermelon, spinach, potato, tomato, radish-root, and water fortified with the herbicides ranged from 63.6 to 107.3% and relative standard deviations were <15.3%.