Determination of Pesticide Residues in Drinking Water Using the LC-MS/MS Method and Evaluation of the Results for 2023 and 2024 †
Abstract
1. Introduction
2. Materials and Methods
2.1. Apparatus and Reagents
2.2. Samples and Sample Pretreatment
2.3. Preparation of Blank, Calibration Solutions and Solution for Recovery
3. Results
3.1. Validation and/or Verification of Method for Pesticide Residues
3.2. Samples Determination
4. Discussion
5. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
- Available online: https://food.ec.europa.eu/plants/pesticides_en (accessed on 8 November 2025).
- Available online: https://www.slov-lex.sk/ezbierky/pravne-predpisy/SK/ZZ/2007/355/ (accessed on 8 November 2025).
- Ministry of Health of the Slovak Republic. Decree No. 91/2023 Coll. on Indicators and Limit Values of Drinking Water Quality. Available online: https://www.slov-lex.sk/pravne-predpisy/SK/ZZ/2023/91/ (accessed on 8 November 2025).
- Available online: https://food.ec.europa.eu/system/files/2016-10/pesticides_ppp_app-proc_guide_fate_metabolites-groundwtr.pdf (accessed on 8 November 2025).
- Available online: https://www.uvzsr.sk/documents/41637/141899/Rozhodnutie_pre_vybrane_nerelevantne_metabolity_pesticidov.pdf/ac7e3fe2-bed2-348d-15ad-93bb410afe01?t=1659890973238 (accessed on 8 November 2025).
- Public Health Authority of the Slovak Republic. List of Pesticides and Relevance of Their Metabolites to Be Analyzed in Drinking Water. Available online: https://www.uvzsr.sk/documents/41637/123252/Pesticidy_Zoznam.pdf/a0973c8f-9b70-0dce-ad65-fd0b68d52980?t=1659284813091 (accessed on 8 November 2025).
- Available online: https://food.ec.europa.eu/document/download/d4786faf-c574-4222-a5c6-45086b3920b8_en?filename=pesticides_mrl_guidelines_wrkdoc_2021-11312.pdf (accessed on 8 November 2025).
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| Pesticide μg/L (LOD 0.020) (LOQ 0.025) | Active Substance/ Metabolite Relevant or Irrelevant | Limit μg/L | Accreditation | % Blank from Minimal Calibration Point | Correlation Coefficient | QC % | Recovery % Nylon | Recovery % H-PTFE |
|---|---|---|---|---|---|---|---|---|
| Acceptation Criteria | <30 | >0.995 | 80–120 | 80–120 | 80–120 | |||
| 2,4-D | active substance | 0.10 * | N | 0.0 | 0.99700 | 93 | <0 | 101 |
| 2,6-Dichlorobenzamide | irrelevant metabolite | 3 | N | 2.2 | 0.99981 | 98 | 99 | 101 |
| Acetochlor ESA | relevant metabolite | 0.10 * | A | 0.0 | 0.99857 | 104 | N/A | 97 |
| Acetochlor OA | relevant metabolite | 0.10 * | A | 5.2 | 0.99978 | 108 | 56 | 100 |
| Acetochlor | active substance (forbidden from 2011) | 0.10 * | A | 0.0 | 0.99899 | 104 | 104 | 89 |
| Alachlor ESA | irrelevant metabolite | 1 ** | A | 0.0 | 0.99666 | 103 | N/A | 101 |
| Alachlor OA | irrelevant metabolite | 1 ** | A | 8.1 | 0.99926 | 99 | 56 | 101 |
| Alachlor | active substance (forbidden from 2007) | 0.10 * | N | 0.0 | 0.99971 | 97 | 83 | 87 |
| Anthranilic acid isopropylamide | 0.10 * | N | 0.0 | 0.99998 | 104 | 105 | 106 | |
| Atrazine | active substance (forbidden from 2005) | 0.10 * | A | 1.6 | 0.99990 | 100 | 100 | 99 |
| Atrazine-2-hydroxy | irrelevant metabolite | 2 ** | N | 0.5 | 0.99998 | 102 | 103 | 105 |
| Atrazine-desethyl | relevant metabolite | 0.10 * | A | 0.0 | 0.99965 | 104 | 103 | 101 |
| Atrazine-desethyl-desisopropyl | relevant metabolite | 0.10 * | N | 0.0 | 0.99758 | 96 | 104 | 100 |
| Atrazine-desisopropyl | relevant metabolite | 0.10 * | N | 0.0 | 0.99997 | 101 | 103 | 107 |
| Azoxystrobin (free acid) | 0.10 * | N | 12.4 | 0.99927 | 106 | 91 | 96 | |
| Azoxystrobin | active substance | 0.10 * | N | 0.0 | 0.99961 | 99 | 92 | 91 |
| Bentazone methyl | metabolite | N | 0.0 | 0.99969 | 100 | 94 | 97 | |
| Bentazone | active substance | 0.10 * | N | 0.0 | 0.99882 | 101 | N/A | 108 |
| Carbendazim | metabolite | 0.10 * | N | 0.0 | 0.99974 | 104 | 102 | 107 |
| Clopyralid | active substance | N | 0.0 | 0.99902 | 110 | 83 | 119 | |
| Cyproconazole | active substance | 0.10 * | N | 0.0 | 0.99985 | 103 | 100 | 103 |
| Desmedipham | active substance | 0.10 * | N | 0.0 | 0.99939 | 101 | N/A | 80 |
| Difenoconazole | N | 0.0 | 0.99975 | 93 | 16 | 88 | ||
| Diflufenican | active substance | 0.10 * | N | 0.0 | 0.99948 | 95 | 14 | 42 |
| Dichlorprop-P | active substance | N | 0.0 | 0.99983 | 94 | <0 | 98 | |
| Dimethachlor ESA | relevant metabolite | 0.10 * | A | 0.0 | 0.99844 | 95 | 69 | 105 |
| Dimethachlor OA | relevant metabolite | 0.10 * | A | 0.0 | 0.99995 | 103 | 97 | 103 |
| Dimethachlor | active substance | 0.10 * | N | 0.0 | 0.99924 | 97 | 60 | 65 |
| Dimethenamid ESA | metabolite | N | 0.0 | 0.99959 | 101 | 42 | 106 | |
| Dimethenamid OA | metabolite | N | 0.0 | 0.99999 | 104 | 83 | 105 | |
| Dimethenamid-P | active substance | 0.0 | 0.99934 | 100 | 98 | 101 | ||
| DMS | N | 0.0 | 0.99997 | 106 | 106 | 82 | ||
| Epoxiconazole | active substance | 0.10 * | N | 0.0 | 0.99835 | 98 | 94 | 100 |
| Ethofumesate | active substance | 0.10 * | N | 0.0 | 0.99696 | 99 | 115 | 101 |
| Fenpropidin | N | 0.0 | 0.99984 | 102 | 93 | 97 | ||
| Flufenacet ESA | metabolite | N | 0.0 | 0.99667 | 101 | 67 | 97 | |
| Flufenacet OA | metabolite | 0.10 * | N | 0.0 | 0.99611 | 113 | 84 | 104 |
| Flufenacet | active substance | 0.10 * | N | 0.0 | 0.99986 | 95 | 105 | 99 |
| Fluopicolide | N | 0.0 | 0.99993 | 95 | 95 | 99 | ||
| Fluroxypyr | active substance | 0.10 * | N | 0.0 | 0.99956 | 105 | 6 | 101 |
| Hexazinone | N | 0.0 | 0.99997 | 101 | 75 | 99 | ||
| Chloridazon | active substance | 0.10 * | N | 0.0 | 0.99919 | 101 | 99 | 103 |
| Chloridazon-desphenyl | irrelevant metabolite | 6 ** | N | 0.0 | 0.99946 | 96 | 112 | 103 |
| Chloridazon-methyl-desphenyl | irrelevant metabolite | 6 ** | N | 0.0 | 0.99987 | 108 | 108 | 108 |
| Chlormequat chloride | active substance | 0.10 * | N | 0.0 | 0.99807 | 93 | 90 | 114 |
| Chlorotoluron | active substance | 0.10 * | N | 0.0 | 0.99876 | 98 | 80 | 98 |
| Chlorotoluron-desmethyl | 0.10 * | N | 0.0 | 0.99670 | 96 | 60 | 89 | |
| Chlorpyrifos | active substance | 0.10 * | N | 0.0 | 0.99971 | 96 | 10 | 49 |
| Chlorsulfuron | active substance | 0.10 * | N | 0.0 | 0.99896 | 98 | 1 | 96 |
| Imidacloprid | N | 0.0 | 0.99985 | 92 | 106 | 112 | ||
| Isoproturon | active substance | 0.10 * | N | 0.0 | 0.99965 | 105 | 98 | 101 |
| Isoproturon-desmethyl | relevant metabolite | 0.10 * | N | 0.0 | 0.99958 | 94 | 99 | 101 |
| Lenacil | active substance | 0.10 * | N | 0.0 | 0.99865 | 117 | 95 | 106 |
| Linuron | active substance (forbidden from 2017) | 0.10 * | N | 0.0 | 0.99954 | 97 | 82 | 100 |
| MCPA | active substance | 0.10 * | N | 0.0 | 0.99976 | 109 | N/A | 93 |
| MCPB | active substance | 0.10 * | N | 0.0 | 0.99823 | 97 | 31 | 118 |
| Mecoprop | active substance | 0.10 * | N | 0.0 | 0.99937 | 91 | <0 | 95 |
| Mesotrione | active substance | 0.10 * | N | 0.0 | 0.99584 | 106 | 52 | 100 |
| Metamitron | active substance | 0.10 * | N | 0.0 | 0.99994 | 100 | 107 | 105 |
| Metazachlor ESA | irrelevant metabolite | 5 ** | N | 0.0 | 0.99937 | 120 | 34 | 103 |
| Metazachlor OA | irrelevant metabolite | 5 ** | A | 0.0 | 0.99889 | 108 | 73 | 96 |
| Metazachlor | active substance | 0.10 * | A | 0.0 | 0.99963 | 101 | 104 | 101 |
| Metolachlor ESA | irrelevant metabolite | 6 ** | N | 0.0 | 0.99986 | 103 | 3 | 87 |
| Metolachlor OA | irrelevant metabolite | 6 ** | N | 0.0 | 0.99814 | 104 | 55 | 105 |
| Metribuzin | active substance | 0.10 * | N | 0.0 | 0.99937 | 109 | 100 | 102 |
| Metribuzin-desamino-diketo | metabolite/relevant | N | 0.0 | 0.99986 | 107 | 125 | 118 | |
| N,N-Dimethyl-2-sulfamoylnicotinamide | 0.10 * | N | 0.0 | 0.99913 | 105 | 106 | 96 | |
| Nicosulfuron | active substance | 0.10 * | N | 0.0 | 0.99995 | 101 | 80 | 108 |
| Parathion-ethyl | N | 0.0 | 0.99735 | 112 | 93 | 80 | ||
| Pendimethalin | active substance | 0.10 * | N | 0.0 | 0.99985 | 97 | 6 | 33 |
| Pethoxamid ESA | metabolite/relevant | N | 0.0 | 0.99922 | 93 | 18 | 88 | |
| Pethoxamid | active substance | 0.10 * | N | 0.0 | 0.99986 | 97 | 98 | 97 |
| Phenmedipham | active substance | 0.10 * | N | 0.0 | 0.99868 | 99 | 1 | 74 |
| Prochloraz | active substance | 0.10 * | N | 0.0 | 0.9994 | 92 | 91 | 102 |
| Prometryn | active substance | 0.10 * | A | 0.0 | 0.99985 | 102 | 102 | 101 |
| Propazine | active substance | 0.10 * | A | 0.0 | 0.99988 | 99 | 100 | 102 |
| Propiconazole | active substance | 0.10 * | N | 0.0 | 0.99989 | 96 | 96 | 95 |
| Prosulfocarb | N | 0.0 | 0.99989 | 96 | 75 | 85 | ||
| Prothioconazole | active substance | N | 0.0 | 0.99714 | 86 | N/A | 70 | |
| Pyraclostrobin | N | 0.0 | 0.99993 | 95 | 1 | 83 | ||
| Quinmerac | active substance | 0.10 * | N | 0.0 | 0.99977 | 103 | 58 | 98 |
| Simazine | active substance (forbidden from 2025) | 0.10 * | A | 0.0 | 0.99990 | 93 | 88 | 104 |
| Simazine-2-hydroxy | metabolite/relevant | N | 0.0 | 0.99995 | 101 | 104 | 105 | |
| S-Metolachlor | active substance | 0.10 * | N | 0.0 | 0.99833 | 98 | 97 | 100 |
| Tebuconazole | active substance | 0.10 * | N | 0.0 | 0.99984 | 94 | 94 | 101 |
| Terbuthylazine | active substance | 0.10 * | A | 0.0 | 0.99995 | 98 | 98 | 99 |
| Terbuthylazine-2-hydroxy | relevant metabolite | 0.10 * | N | 0.0 | 0.99974 | 104 | 106 | 104 |
| Terbuthylazine-desethyl | relevant metabolite | 0.10 * | A | 0.0 | 0.99994 | 98 | 92 | 102 |
| Terbuthylazine-desethyl-2-hydroxy | relevant metabolite | 0.10 * | N | 0.0 | 0.99993 | 103 | 104 | 106 |
| Terbutryn | active substance | 0.10 * | N | 0.0 | 0.99998 | 100 | 97 | 98 |
| Thiabendazole | N | 0.0 | 0.99999 | 102 | 101 | 107 | ||
| Thiophanate-methyl | 0.10 * | N | 0.0 | 0.99990 | 100 | 72 | 104 | |
| LC Conditions | |
|---|---|
| Column: | Kinetex® (Phenomenex, Torrance, CA, USA) 2.6 μm Polar C18 100 Å, 100 × 2.1 mm |
| Column temperature: | 30 °C |
| Injection volume: | 20 μL |
| Autosampler temperature: | 15 °C |
| Mobile phase A: | 0.1% Formic acid in deionized water |
| Mobile phase B: | Methanol |
| Run time: | 17 min |
| Flow rate: | 0.2 mL/min |
| Time (min) | Mobile Phase A (%) | Mobile Phase B (%) |
|---|---|---|
| 0 | 95 | 5 |
| 2 | 95 | 5 |
| 6 | 55 | 45 |
| 10 | 5 | 95 |
| 13 | 5 | 95 |
| 13.05 | 0 | 100 |
| 17 | 0 | 100 |
| MS/MS Conditions | |
|---|---|
| Scan type: | Scheduled MRM |
| Target cycle time: | 1 s |
| Ion source: | ESI |
| Curtain gas (CUR): | 40 psi |
| Collision gas (CAD): | Medium |
| Ion Spray Voltage (IS): | 5500 V |
| Temperature (TEM): | 400 °C |
| Ion source Gas 1 (GS1): | 50 psi |
| Ion source Gas 2 (GS2): | 50 psi |
| Entrance Potential (EP): | 10 V |
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Kuzniarová, M.; Dömötörová, M.; Micháliková, M.; Lukačovičová, Z. Determination of Pesticide Residues in Drinking Water Using the LC-MS/MS Method and Evaluation of the Results for 2023 and 2024. Chem. Proc. 2025, 19, 3. https://doi.org/10.3390/chemproc2025019003
Kuzniarová M, Dömötörová M, Micháliková M, Lukačovičová Z. Determination of Pesticide Residues in Drinking Water Using the LC-MS/MS Method and Evaluation of the Results for 2023 and 2024. Chemistry Proceedings. 2025; 19(1):3. https://doi.org/10.3390/chemproc2025019003
Chicago/Turabian StyleKuzniarová, Miroslava, Milena Dömötörová, Martina Micháliková, and Zuzana Lukačovičová. 2025. "Determination of Pesticide Residues in Drinking Water Using the LC-MS/MS Method and Evaluation of the Results for 2023 and 2024" Chemistry Proceedings 19, no. 1: 3. https://doi.org/10.3390/chemproc2025019003
APA StyleKuzniarová, M., Dömötörová, M., Micháliková, M., & Lukačovičová, Z. (2025). Determination of Pesticide Residues in Drinking Water Using the LC-MS/MS Method and Evaluation of the Results for 2023 and 2024. Chemistry Proceedings, 19(1), 3. https://doi.org/10.3390/chemproc2025019003
