An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry
The presence of pesticide residues in water is a huge worldwide concern. In this paper we described the development and validation of a new liquid chromatography tandem mass spectrometric (LC-MS/MS) method for both screening and quantification of pesticides in water samples. In the sample preparatio...
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| Format: | Article |
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MDPI AG
2022-03-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/27/6/1872 |
| _version_ | 1797444325789925376 |
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| author | Edgár Tóth Ádám Tölgyesi Andrea Simon Mária Bálint Xingmao Ma Virender K. Sharma |
| author_facet | Edgár Tóth Ádám Tölgyesi Andrea Simon Mária Bálint Xingmao Ma Virender K. Sharma |
| author_sort | Edgár Tóth |
| collection | DOAJ |
| description | The presence of pesticide residues in water is a huge worldwide concern. In this paper we described the development and validation of a new liquid chromatography tandem mass spectrometric (LC-MS/MS) method for both screening and quantification of pesticides in water samples. In the sample preparation stage, the samples were buffered to pH 7.0 and pre-concentrated on polymeric-based cartridges via solid-phase extraction (SPE). Highly sensitive detection was carried out with mobile phases containing only 5 mM ammonium formate (pH of 6.8) as an eluent additive and using only positive ionization mode in MS/MS instrument. Hence, only 200-fold sample enrichment was required to set a screening detection limit (SDL) and reporting limit (RL) of 10 ng/L. The confirmatory method was validated at 10 and 100 ng/L spiking levels. The apparent recoveries obtained from the matrix-matched calibration (5–500 ng/L) were within the acceptable range (60–120%), also the precision (relative standard deviation, RSD) was not higher than 20%. During the development, 480 pesticides were tested and 330 compounds fulfilled the requirements of validation. The method was successfully applied to proficiency test samples to evaluate its accuracy. Moreover, the method robustness test was carried out using higher sample volume (500 mL) followed by automated SPE enrichment. Finally, the method was used to analyze 20 real samples, in which some compounds were detected around 10 ng/L, but never exceeded the assay maximum level. |
| first_indexed | 2024-03-09T13:10:58Z |
| format | Article |
| id | doaj.art-ce6f94f88d214058b403a03d20c5ab8e |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-09T13:10:58Z |
| publishDate | 2022-03-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-ce6f94f88d214058b403a03d20c5ab8e2023-11-30T21:42:32ZengMDPI AGMolecules1420-30492022-03-01276187210.3390/molecules27061872An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass SpectrometryEdgár Tóth0Ádám Tölgyesi1Andrea Simon2Mária Bálint3Xingmao Ma4Virender K. Sharma5Bálint Analitika Ltd., Fehérvári út 144, 1116 Budapest, HungaryBálint Analitika Ltd., Fehérvári út 144, 1116 Budapest, HungaryBálint Analitika Ltd., Fehérvári út 144, 1116 Budapest, HungaryBálint Analitika Ltd., Fehérvári út 144, 1116 Budapest, HungaryDepartment of Civil and Environmental Engineering, Texas A&M University, College Station, TX 77843, USAProgram for the Environment and Sustainability, Department of Environmental and Occupational Health, School of Public Health, Texas A&M University, 212 Adriance Lab Road, 1266 TAMU, College Station, TX 77843, USAThe presence of pesticide residues in water is a huge worldwide concern. In this paper we described the development and validation of a new liquid chromatography tandem mass spectrometric (LC-MS/MS) method for both screening and quantification of pesticides in water samples. In the sample preparation stage, the samples were buffered to pH 7.0 and pre-concentrated on polymeric-based cartridges via solid-phase extraction (SPE). Highly sensitive detection was carried out with mobile phases containing only 5 mM ammonium formate (pH of 6.8) as an eluent additive and using only positive ionization mode in MS/MS instrument. Hence, only 200-fold sample enrichment was required to set a screening detection limit (SDL) and reporting limit (RL) of 10 ng/L. The confirmatory method was validated at 10 and 100 ng/L spiking levels. The apparent recoveries obtained from the matrix-matched calibration (5–500 ng/L) were within the acceptable range (60–120%), also the precision (relative standard deviation, RSD) was not higher than 20%. During the development, 480 pesticides were tested and 330 compounds fulfilled the requirements of validation. The method was successfully applied to proficiency test samples to evaluate its accuracy. Moreover, the method robustness test was carried out using higher sample volume (500 mL) followed by automated SPE enrichment. Finally, the method was used to analyze 20 real samples, in which some compounds were detected around 10 ng/L, but never exceeded the assay maximum level.https://www.mdpi.com/1420-3049/27/6/1872pesticideswatersolid-phase extractionLC-MS/MSvalidation |
| spellingShingle | Edgár Tóth Ádám Tölgyesi Andrea Simon Mária Bálint Xingmao Ma Virender K. Sharma An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry Molecules pesticides water solid-phase extraction LC-MS/MS validation |
| title | An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry |
| title_full | An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry |
| title_fullStr | An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry |
| title_full_unstemmed | An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry |
| title_short | An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry |
| title_sort | alternative strategy for screening and confirmation of 330 pesticides in ground and surface water using liquid chromatography tandem mass spectrometry |
| topic | pesticides water solid-phase extraction LC-MS/MS validation |
| url | https://www.mdpi.com/1420-3049/27/6/1872 |
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