PMID- 31307794
OWN - NLM
STAT- MEDLINE
DCOM- 20200113
LR  - 20231213
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1605
DP  - 2019 Nov 8
TI  - Robust and highly sensitive micro liquid chromatography-tandem mass spectrometry 
      method for analyses of polar pesticides (glyphosate, aminomethylphosfonic acid, 
      N-acetyl glyphosate and N-acetyl aminomethylphosfonic acid) in multiple 
      biological matrices.
PG  - 360343
LID - S0021-9673(19)30673-9 [pii]
LID - 10.1016/j.chroma.2019.06.064 [doi]
AB  - Glyphosate is the most used herbicide in agriculture. To monitor glyphosate 
      exposure, analytical methods have to fulfill requirements with regard to 
      sensitivity, reproducibility, ease of handling/high-throughput and applicability 
      to multiple biological matrices. Furthermore, the methods have to include the 
      degradation product of glyphosate, aminomethylphosfonic acid (AMPA) and 
      preferably metabolites of glyphosate and AMPA, N-acetyl AMPA and N-acetyl 
      glyphosate. Majority of the published methods for glyphosate and AMPA require 
      derivatization to be able to achieve high sensitivity. In this work, we present 
      highly sensitive microLC-MS/MS method for simultaneous quantification of 
      glyphosate, AMPA, N-acetyl AMPA and N-acetyl glyphosate in multiple biological 
      matrices without derivatization. The combination of simple sample clean-up 
      procedures for simultaneous handling of 96 sample and short chromatographic run 
      of only 3.4 min, meets the requirements for high-throughput methods. Simple 
      mobile phase of water containing formic and medronic acids and isocratic run 
      provided robust chromatographic separation on hypercarb column. The use of 
      micro-flow system decreased the background noise, increasing the sensitivity. 
      Achieved Low Limits of Quantification (LOQs) for liquid samples 
      (plasma/serum/urine) were 0.00005 mg L(-1) and 0.0001 mg kg(-1) for solid samples 
      (grain and soybean based feed/stomach/gizzard/intestinal content), which is more 
      than 100 time more sensitive compared to QuPPe-Method. The method was validated 
      in representative matrices with minimum of five fortification levels, six 
      measurements per spiked concentration and three batches. All the samples were 
      spiked with corresponding internal standards for all four analytes before sample 
      clean-up procedures, ensuring high accuracy and precision. Recoveries for 
      plasma/serum ranged between 86-108%, urine 93-120%, feed 91-115% and 
      stomach/gizzard/intestinal content 92-110% with precision below 20%. The method's 
      applicability was tested on 2000 samples measured during one year period.
CI  - Copyright (c) 2019 Elsevier B.V. All rights reserved.
FAU - Norskov, Natalja P
AU  - Norskov NP
AD  - Department of Animal Science, Aarhus University, Blichers Alle 20, DK-8830, 
      Denmark. Electronic address: Natalja.Norskov@anis.au.dk.
FAU - Jensen, Soren Krogh
AU  - Jensen SK
AD  - Department of Animal Science, Aarhus University, Blichers Alle 20, DK-8830, 
      Denmark.
FAU - Sorensen, Martin Tang
AU  - Sorensen MT
AD  - Department of Animal Science, Aarhus University, Blichers Alle 20, DK-8830, 
      Denmark.
LA  - eng
PT  - Journal Article
DEP - 20190702
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Pesticides)
RN  - 059QF0KO0R (Water)
RN  - TE7660XO1C (Glycine)
SB  - IM
MH  - *Chromatography, Liquid
MH  - Glycine/analogs & derivatives
MH  - Pesticides/*analysis
MH  - Reproducibility of Results
MH  - *Tandem Mass Spectrometry
MH  - Water/chemistry
MH  - Glyphosate
OTO - NOTNLM
OT  - Aminomethylphosphonic acid
OT  - Glyphosate
OT  - Metabolites
OT  - MicroLC-MS/MS
OT  - Solid-phase extraction
EDAT- 2019/07/17 06:00
MHDA- 2020/01/14 06:00
CRDT- 2019/07/17 06:00
PHST- 2019/04/10 00:00 [received]
PHST- 2019/06/28 00:00 [revised]
PHST- 2019/06/29 00:00 [accepted]
PHST- 2019/07/17 06:00 [pubmed]
PHST- 2020/01/14 06:00 [medline]
PHST- 2019/07/17 06:00 [entrez]
AID - S0021-9673(19)30673-9 [pii]
AID - 10.1016/j.chroma.2019.06.064 [doi]
PST - ppublish
SO  - J Chromatogr A. 2019 Nov 8;1605:360343. doi: 10.1016/j.chroma.2019.06.064. Epub 
      2019 Jul 2.