Method validation and application of a selective multiresidue analysis of highly polar pesticides in food matrices using hydrophilic interaction liquid chromatography and mass spectrometry

López, Sonia Herrera; Scholten, Jos; Kiedrowska, Barbara; Kok, Albert

doi:10.1016/j.chroma.2019.02.024

Cited by 50 publications

(20 citation statements)

References 19 publications

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“…As it can be observed, liquid chromatography is particularly appropriate for the analysis of polar, non-volatile, and/or thermally labile pesticides. Because of its high selectivity and sensitivity, HPLC and UHPLC in combination with MS/MS have mostly been used in this field especially to determine the insecticides and herbicides belonging to organophosphorus compounds, imidazolinone and pyridine carboxylic acid derivatives, and in study of samples containing multiclass pesticides [16][17][18][19][20][21][22][23][24]27,[30][31][32][33][34]. However, in a few cases, i.e., triazine and phenylurea herbicides, the HPLC coupled with spectrophotometric detection HPLC-UV or DAD has also been applied [25,26,28].…”

Section: Column Liqiud Chromatography In Analysis Of Selected Bioactive Compounds In Food Samplesmentioning

confidence: 99%

“…However, in a few cases, i.e., triazine and phenylurea herbicides, the HPLC coupled with spectrophotometric detection HPLC-UV or DAD has also been applied [25,26,28]. Various kinds of stationary phases (columns) have been used in the HPLC determination of pesticides, mainly C18 [16][17][18]20,[25][26][27][28][29][30][31], and also chiral [19,33], BEH HILIC [21], Hypercarb [22], Obelisc N HILIC [24,34], Acquity UPLC HSS T3 [23,32]. In general, water or water with formic acid or acetic acid or ammonium formate, acetonitrile, and methanol have been applied as mobile phases with gradient or isocratic elution, respectively.…”

Section: Column Liqiud Chromatography In Analysis Of Selected Bioactive Compounds In Food Samplesmentioning

confidence: 99%

“…As is shown in Table 1, many HPLC-MS/MS techniques with triple quadrupole (TQ), electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode or selected reaction monitoring (SRM) mode have been mainly used for the determination of different kind of pesticides [16,[18][19][20][21]27,31,33]. In addition, the HPLC-MS/MS methods with electrospray ionization (ESI) and quadrupole trap (QTRAP) in multiple reaction monitoring (MRM) mode have been also employed in the analysis of various pesticides [23,24,30,34]. Whereas UHPLC-Q Orbitrap-ESI-MS/MS has been applied for the determination of highly polar pesticides and contaminants (glyphosate, aminomethyl phosphonic acid (AMPA), phosphonic acid, fosetyl-Al, chlorate, and perchlorate) in processed fruits, vegetables, and infant foods [22].…”

Section: Column Liqiud Chromatography In Analysis Of Selected Bioactive Compounds In Food Samplesmentioning

confidence: 99%

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Current Strategies for Studying the Natural and Synthetic Bioactive Compounds in Food by Chromatographic Separation Techniques

2021

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The present study summarizes the new strategies including advanced equipment and validation parameters of liquid and gas chromatography methods i.e., thin-layer chromatography (TLC), column liquid chromatography (CLC), and gas chromatography (GC) suitable for the identification and quantitative determination of different natural and synthetic bioactive compounds present in food and food products, which play an important role in human health, within the period of 2019–2021 (January). Full characteristic of some of these procedures with their validation parameters is discussed in this work. The present review confirms the vital role of HPLC methodology in combination with different detection modes i.e., HPLC-UV, HPLC-DAD, HPLC-MS, and HPLC-MS/MS for the determination of natural and synthetic bioactive molecules for different purposes i.e., to characterize the chemical composition of food as well as in the multi-residue analysis of pesticides, NSAIDs, antibiotics, steroids, and others in food and food products.

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Section: Column Liqiud Chromatography In Analysis Of Selected Bioactive Compounds In Food Samplesmentioning

confidence: 99%

Section: Column Liqiud Chromatography In Analysis Of Selected Bioactive Compounds In Food Samplesmentioning

confidence: 99%

Section: Column Liqiud Chromatography In Analysis Of Selected Bioactive Compounds In Food Samplesmentioning

confidence: 99%

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Current Strategies for Studying the Natural and Synthetic Bioactive Compounds in Food by Chromatographic Separation Techniques

2021

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“…In order to simplify and to fast the monitoring of GLY and AMPA, researchers have addressed the development of more efficient and/or selective extraction procedures, such as molecularly imprinted polymers (MIP), so far tested for extraction and concentration of GLY from water samples [ 10 ]; strategies to mask the ligand character of GLY and AMPA [ 11 ]; and particularly, novel stationary phases (based on hydrophilic interactions, HILIC [ 12 , 13 ], ionic exchange [ 14 , 15 ], or mixed-mode columns [ 16 ]) in LC improving the retention of these compounds and permitting the use of mobile phases compatible with electrospray ionization, previously to their mass spectrometry detection (ESI–MS).…”

Section: Introductionmentioning

confidence: 99%

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

et al. 2021

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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

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“…Furthermore, many literature reports describe that glyphosate and its co-formulants (used in pesticides) can be included in the group of compounds that cause the endocrine effect [8,[10][11][12][13][14][15][16][17][18][19][20][21]. However, the regulations regarding these compounds are constantly changing.…”

Section: Introductionmentioning

confidence: 99%

Determination of Glyphosate and AMPA in Food Samples Using Membrane Extraction Technique for Analytes Preconcentration

2021

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The method for determining glyphosate (NPG) and its metabolite AMPA (aminomethyl phosphonic acid) in solid food samples using UAE-SLM-HPLC–PDA technique was developed. Firstly, ultrasonic-assisted solvent extraction (UAE) and protein precipitation step were used for the analyte isolation. Then, the supernatant was evaporated to dryness and redissolved in distilled water (100 mL). The obtained solution was alkalized to pH 11 (with 1 M NaOH) and used directly as donor phase in SLM (supported liquid membrane) extraction. The SLM extraction was performed using 2 M NaCl (5 mL) as an acceptor phase. The flow rate of both phases (donor and acceptor) was set at 0.2 mL/min. The membrane extraction took 24 h but did not require any additional workload. Finally, the SLM extracts were analyzed using the HPLC technique with photo-diode array detector (PDA) and an application of pre-column derivatization with p-toluenesulfonyl chloride. Glyphosate residues were determined in food samples of walnuts, soybeans, barley and lentil samples. The LOD values obtained for the studied food were 0.002 μg g−1 and 0.021 μg g−1 for NPG and AMPA, respectively. Recoveries values ranged from 32% to 69% for NPG, 29% to 56% for AMPA and depended on the type of sample matrix. In the case of buckwheat and rice flour samples, the content of NPG and AMPA was below the detection level of a used analytical method.

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Method validation and application of a selective multiresidue analysis of highly polar pesticides in food matrices using hydrophilic interaction liquid chromatography and mass spectrometry

Cited by 50 publications

References 19 publications

Current Strategies for Studying the Natural and Synthetic Bioactive Compounds in Food by Chromatographic Separation Techniques

Current Strategies for Studying the Natural and Synthetic Bioactive Compounds in Food by Chromatographic Separation Techniques

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

Determination of Glyphosate and AMPA in Food Samples Using Membrane Extraction Technique for Analytes Preconcentration

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