Development of a sensitive direct injection LC-MS/MS method for the detection of glyphosate and aminomethylphosphonic acid (AMPA) in hard waters

Ulrich, Jake C.; Ferguson, P. Lee

doi:10.1007/s00216-021-03324-5

Cited by 21 publications

(17 citation statements)

References 47 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…However, these can still suffer limited selectivity for application to large numbers of chemically diverse CECs as well as the potential for analyte and matrix carryover if the methods are not properly optimised, especially in complex samples. While direct-injection MS methods are still not widely considered for the quantitation of large numbers of CECs due to the potential for significant matrix effects, recently, direct-injection LC-MS of CECs in water has emerged, usually with gradient pre-separation to minimise these effects [6][7][8][9][10][11][12][13][14]. In many cases, this requires the large volume injection (LVI) of sample (typically between 80-5000 µL) and can help overcome the issue of analyte selectivity loss during pre-treatment.…”

Section: Introductionmentioning

confidence: 99%

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography—Tandem Mass Spectrometry

et al. 2021

View full text Add to dashboard Cite

The rapid source identification and environmental risk assessment (ERA) of hundreds of chemicals of emerging concern (CECs) in river water represent a significant analytical challenge. Herein, a potential solution involving a rapid direct-injection liquid chromatography–tandem mass spectrometry method for the quantitative determination of 102 CECs (151 qualitatively) in river water is presented and applied across six rivers in Germany and Switzerland at high spatial resolution. The method required an injection volume of only 10 µL of filtered sample, with a runtime of 5.5 min including re-equilibration with >10 datapoints per peak per transition (mostly 2 per compound), and 36 stable isotope-labelled standards. Performance was excellent from the low ng/L to µg/L concentration level, with 260 injections possible in any 24 h period. The method was applied in three separate campaigns focusing on the ERA of rivers impacted by wastewater effluent discharges (1 urban area in the Basel city region with 4 rivers, as well as 1 semi-rural and 1 rural area, each focusing on 1 river). Between 25 and 40 compounds were quantified directly in each campaign, and in all cases small tributary rivers showed higher CEC concentrations (e.g., up to ~4000 ng/L in total in the R. Schwarzach, Bavaria, Germany). The source of selected CECs could also be identified and differentiated from other sources at pre- and post- wastewater treatment plant effluent discharge points, as well as the effect of dilution downstream, which occurred over very short distances in all cases. Lastly, ERA for 41 CECs was performed at specific impacted sites, with risk quotients (RQs) at 1 or more sites estimated as high risk (RQ > 10) for 1 pharmaceutical (diclofenac), medium risk (RQ of 1–10) for 3 CECs (carbamazepine, venlafaxine, and sulfamethoxazole), and low risk (RQ = 0.1–1.0) for 7 CECs (i.e., RQ > 0.1 for 11 CECs in total). The application of high-throughput methods like this could enable a better understanding of the risks of CECs, especially in low flow/volume tributary rivers at scale and with high resolution.

show abstract

Section: Introductionmentioning

confidence: 99%

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography—Tandem Mass Spectrometry

et al. 2021

View full text Add to dashboard Cite

show abstract

“…2B and C ) considering mobile phase compositions and gradients compiled in Table S1 . Selected columns and mobile phases have been previously reported for AMPA and GLY determination in water samples [ 15 , 22 ]. In the three cases, separations were carried out in the same LC–ESI–MS/MS instrument, under identical conditions as regards ESI parameters and MRM transitions (Table 3 ).…”

Section: Resultsmentioning

confidence: 99%

Approaches to liquid chromatography tandem mass spectrometry assessment of glyphosate residues in wine

et al. 2021

View full text Add to dashboard Cite

The performance of two different analytical methodologies to investigate the presence of glyphosate (GLY) and aminomethylphosphonic acid (AMPA) residues in wine samples was evaluated. Transformation of compounds in their fluorene-9-methyloxycarbonyl derivatives permitted their separation under reversed-phase liquid chromatography with tandem mass spectrometry (LC–MS/MS) determination. Although the wine matrix severely impaired the efficiency of GLY derivatization, this drawback was solved using a molecularly imprinted sorbent for the previous, selective extraction of GLY and AMPA from wine. Alternatively, the use of a strong anionic exchange, polyvinyl alcohol-based LC column, turned to be the most effective alternative for direct determination of both compounds in diluted wine samples. The chromatographic behavior of this column and the magnitude of matrix effects observed during analysis of diluted wine samples were significantly affected by the composition of the mobile phase. Under final working conditions, this column permitted the separation of AMPA and the fungicide fosetyl (which shows common transitions in tandem MS/MS methods), it improved significantly the sample throughput versus extraction-derivatization-purification method, and it allowed the use of solvent-based calibration standards. Both analytical procedures provided similar limits of quantification (LOQs) for GLY (0.5–1.0 ng mL−1), while the multistep method was 8 times more sensitive to AMPA than the direct procedure. GLY residues stayed above method LOQs in 70% of the processed wines; however, concentrations measured in 95% of positive samples remained 100 times below the maximum residue limit (MRL) set for GLY in vinification grapes. Graphical abstract

show abstract

“…8–10 Although glyphosate is a non-electroactive compound and cannot be measured at an accessible potential, there have been reports of electrochemical sensing of glyphosate by modifying the electrode and processing the sample. 11–13 Prasad et al 14 constructed an electrochemical sensor based on a graphite electrode modified by a dual-template imprinted polymer nanomembrane and used it to detect glyphosate in soil. The linear response range and the limit of detection of the sensor to glyphosate are 3.98–176.23 ng ml −1 and 0.35 ng ml −1 , respectively.…”

Section: Introductionmentioning

confidence: 99%

A novel electrochemical sensor for glyphosate detection based on Ti₃C₂T_x/Cu-BTC nanocomposite

et al. 2022

View full text Add to dashboard Cite

show abstract

Development of a sensitive direct injection LC-MS/MS method for the detection of glyphosate and aminomethylphosphonic acid (AMPA) in hard waters

Cited by 21 publications

References 47 publications

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography—Tandem Mass Spectrometry

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography—Tandem Mass Spectrometry

Approaches to liquid chromatography tandem mass spectrometry assessment of glyphosate residues in wine

A novel electrochemical sensor for glyphosate detection based on Ti₃C₂T_x/Cu-BTC nanocomposite

Contact Info

Product

Resources

About

Development of a sensitive direct injection LC-MS/MS method for the detection of glyphosate and aminomethylphosphonic acid (AMPA) in hard waters

Cited by 21 publications

References 47 publications

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography—Tandem Mass Spectrometry

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography—Tandem Mass Spectrometry

Approaches to liquid chromatography tandem mass spectrometry assessment of glyphosate residues in wine

A novel electrochemical sensor for glyphosate detection based on Ti3C2Tx/Cu-BTC nanocomposite

Contact Info

Product

Resources

About

A novel electrochemical sensor for glyphosate detection based on Ti₃C₂T_x/Cu-BTC nanocomposite