Determination of Pesticide Residues in Olive Oil Using QuEChERS Extraction and Liquid Chromatography–Orbitrap High-Resolution Mass Spectrometry: Comparison of Different Clean-Up Sorbents and Validation Study
Abstract
:1. Introduction
2. Materials and Methods
3. Results and Discussion
3.1. Identification and Quantification of the Target Pesticides by UHPLC-Orbitrap-MS
3.2. Clean-Up Optimization
3.3. Method Validation
3.3.1. Accuracy, Precision and Repeatability
3.3.2. Linearity, ME, LOQs, LODs and Method Uncertainty
4. Discussion
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Intra-Day | Inter-Day | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
30 μg/kg | 100 μg/kg | 300 μg/kg | 30 μg/kg | 100 μg/kg | 300 μg/kg | |||||||
%Rec | RSDr | %Rec | RSDr | %Rec | RSDr | %Rec | RSDR | %Rec | RSDR | %Rec | RSDR | |
Alachlor | 83.11 | 8.01 | 83.88 | 3.53 | 92.41 | 5.11 | 70.46 | 14.02 | 70.72 | 6.15 | 89.61 | 5.01 |
Azoxystrobin | 90.51 | 3.71 | 98.87 | 2.47 | 101.70 | 3.59 | 77.44 | 16.54 | 80.59 | 11.61 | 105.45 | 4.10 |
Benalaxyl | 72.14 | 4.86 | 92.03 | 2.00 | 99.86 | 4.73 | 72.12 | 2.91 | 75.76 | 13.52 | 103.66 | 3.70 |
Boscalid | 79.09 | 6.53 | 83.56 | 1.83 | 91.47 | 2.82 | 72.07 | 1.61 | 73.10 | 9.93 | 94.28 | 3.32 |
Chlorfenviphos | 101.49 | 5.50 | 109.13 | 2.22 | 107.11 | 5.61 | 84.29 | 17.53 | 91.39 | 12.38 | 110.95 | 5.21 |
Chlorpyrifos | 79.81 | 3.68 | 58.99 | 2.82 | 73.72 | 5.72 | 74.60 | 10.05 | 53.33 | 10.90 | 73.81 | 8.16 |
Diazinon | 107.22 | 5.15 | 122.74 | 1.27 | 115.75 | 5.30 | 99.80 | 16.66 | 102.70 | 10.95 | 119.16 | 4.26 |
Difenoconazole | 75.56 | 4.89 | 70.31 | 2.35 | 81.07 | 5.65 | 89.59 | 23.10 | 70.08 | 11.97 | 83.13 | 3.71 |
Dimethoate | 92.68 | 2.42 | 99.24 | 2.04 | 105.62 | 3.07 | 81.98 | 14.48 | 80.44 | 12.41 | 108.71 | 4.25 |
Diuron | 77.83 | 3.50 | 78.29 | 2.62 | 89.63 | 2.91 | 73.13 | 6.30 | 74.73 | 11.39 | 73.13 | 6.30 |
Fenbuconazole | 78.53 | 9.16 | 84.21 | 2.20 | 95.50 | 3.93 | 72.42 | 10.83 | 72.24 | 12.86 | 95.06 | 4.89 |
Fenoxycarb | 74.56 | 7.35 | 82.59 | 2.19 | 97.50 | 4.50 | 70.32 | 4.81 | 70.36 | 9.07 | 98.00 | 4.46 |
Florasulam | 102.99 | 5.35 | 75.58 | 7.80 | 83.52 | 4.99 | 88.73 | 10.32 | 72.27 | 14.10 | 90.68 | 6.67 |
Fluquinconazole | 86.11 | 8.68 | 81.76 | 1.65 | 86.42 | 3.11 | 75.79 | 14.79 | 76.05 | 12.96 | 88.16 | 7.05 |
Iodosulfuron methyl | 23.50 | 4.87 | 23.08 | 7.47 | 71.15 | 6.71 | 22.64 | 21.11 | 22.80 | 8.98 | 85.10 | 5.83 |
Imazalil | 40.25 | 17.17 | 54.07 | 8.88 | 65.27 | 4.86 | 43.94 | 20.45 | 45.54 | 7.46 | 68.32 | 3.33 |
Deltamethin | 82.34 | 13.39 | 58.17 | 8.20 | 80.60 | 1.67 | 70.20 | 11.25 | 42.65 | 13.06 | 86.59 | 12.16 |
Trifloxystrobin | 92.46 | 5.85 | 99.41 | 0.70 | 99.80 | 5.04 | 77.77 | 17.34 | 82.56 | 11.95 | 103.65 | 5.00 |
Isoproturon | 83.99 | 6.29 | 85.13 | 2.93 | 91.55 | 2.30 | 73.00 | 11.53 | 72.65 | 13.33 | 94.00 | 4.20 |
Kresoxim-methyl | 81.50 | 6.54 | 90.77 | 1.56 | 99.14 | 5.26 | 75.73 | 5.95 | 73.51 | 11.58 | 102.82 | 5.03 |
Metalaxyl | 93.55 | 1.82 | 99.28 | 2.67 | 102.51 | 3.75 | 84.77 | 18.61 | 83.72 | 10.72 | 107.54 | 4.02 |
Myclobutanil | 80.94 | 8.73 | 86.44 | 1.27 | 92.84 | 5.02 | 79.95 | 7.92 | 70.60 | 13.20 | 97.68 | 3.52 |
Mefenpyr-diethyl | 104.08 | 4.13 | 109.31 | 1.86 | 101.72 | 4.49 | 88.23 | 17.98 | 91.86 | 11.57 | 105.36 | 3.76 |
Nicosulfuron | 92.33 | 6.93 | 42.92 | 21.98 | 52.64 | 3.59 | 83.85 | 11.86 | 49.82 | 10.88 | 58.28 | 8.38 |
Pirimicarb | 80.08 | 3.80 | 86.98 | 3.89 | 99.70 | 3.22 | 77.05 | 4.54 | 71.63 | 11.24 | 101.40 | 3.07 |
Penoxsulam | 82.03 | 5.15 | 74.18 | 7.00 | 83.77 | 4.21 | 72.49 | 12.44 | 68.09 | 12.12 | 87.77 | 5.91 |
Phosmet | 89.77 | 2.62 | 90.14 | 1.67 | 98.17 | 3.49 | 80.41 | 9.10 | 72.53 | 12.90 | 100.71 | 3.07 |
Pyriproxyfen | 40.47 | 3.63 | 52.68 | 3.81 | 59.63 | 2.21 | 34.35 | 19.46 | 42.41 | 15.79 | 58.20 | 3.33 |
Pyraclostrobin | 89.51 | 5.99 | 96.90 | 1.17 | 95.73 | 4.99 | 75.75 | 18.85 | 81.36 | 11.77 | 101.58 | 3.60 |
Quizalofop-p-ethyl | 63.46 | 4.06 | 72.32 | 2.29 | 82.18 | 5.68 | 56.49 | 1.17 | 72.38 | 12.54 | 84.75 | 5.39 |
Spinetoram | 19.35 | 7.16 | 14.16 | 19.94 | 18.47 | 16.88 | 20.64 | 4.14 | 14.62 | 11.24 | 20.96 | 18.53 |
Spirotetramat | 88.85 | 7.48 | 91.18 | 2.60 | 97.84 | 4.76 | 72.52 | 21.39 | 76.87 | 14.63 | 101.57 | 5.05 |
Terbuthylazine | 73.56 | 2.15 | 78.16 | 2.12 | 85.14 | 3.71 | 73.12 | 2.49 | 74.37 | 11.21 | 87.95 | 2.65 |
Thiabendazole | 80.10 | 1.44 | 60.76 | 7.03 | 73.73 | 9.13 | 62.17 | 0.86 | 62.74 | 10.29 | 80.22 | 4.97 |
Thiamethoxam | 103.25 | 2.34 | 89.52 | 2.56 | 96.72 | 3.51 | 94.31 | 10.37 | 71.73 | 13.37 | 100.01 | 4.26 |
Tebuconazole | 80.44 | 3.16 | 68.65 | 5.55 | 83.46 | 4.51 | 63.68 | 1.33 | 66.05 | 12.68 | 84.62 | 4.90 |
Thiacloprid | 94.78 | 4.64 | 98.27 | 5.67 | 101.49 | 2.81 | 80.59 | 12.54 | 77.97 | 11.19 | 101.67 | 3.90 |
Tribenuron-methyl | 82.34 | 3.33 | 85.60 | 1.36 | 95.70 | 2.67 | 71.62 | 14.99 | 71.03 | 15.47 | 96.47 | 2.86 |
λ-cyhalothrin | 101.33 | 4.07 | 76.11 | 8.45 | 95.92 | 17.41 | 84.10 | 10.57 | 64.29 | 5.35 | 102.69 | 15.97 |
Intra-Day | Inter-Day | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
30 μg/kg | 100 μg/kg | 300 μg/kg | 30 μg/kg | 100 μg/kg | 300 μg/kg | |||||||
%Rec | RSDr | %Rec | RSDr | %Rec | RSDr | %Rec | RSDR | %Rec | RSDR | %Rec | RSDR | |
Alachlor | 104.51 | 3.38 | 90.34 | 2.71 | 92.81 | 1.88 | 99.11 | 4.36 | 88.81 | 7.83 | 88.58 | 7.17 |
Azoxystrobin | 97.43 | 2.72 | 107.69 | 3.74 | 105.28 | 2.68 | 98.92 | 3.92 | 105.78 | 7.82 | 103.42 | 4.52 |
Benalaxyl | 74.00 | 3.49 | 77.98 | 4.43 | 97.29 | 3.63 | 74.26 | 5.15 | 77.61 | 6.01 | 95.74 | 4.24 |
Boscalid | 111.61 | 2.78 | 90.02 | 3.06 | 94.16 | 2.46 | 109.57 | 5.00 | 92.49 | 6.52 | 90.07 | 4.24 |
Chlorfenviphos | 81.23 | 5.56 | 112.66 | 5.00 | 103.93 | 3.78 | 79.59 | 3.37 | 109.97 | 5.81 | 103.63 | 2.93 |
Chlorpyrifos | 83.76 | 4.43 | 65.65 | 4.46 | 69.05 | 3.61 | 81.13 | 7.24 | 62.37 | 8.26 | 69.37 | 6.04 |
Diazinon | 111.00 | 2.20 | 121.36 | 2.87 | 112.24 | 4.72 | 109.34 | 2.92 | 121.48 | 5.48 | 111.80 | 3.10 |
Difenoconazole | 81.32 | 5.57 | 86.74 | 5.03 | 98.78 | 3.69 | 79.82 | 6.71 | 83.16 | 5.06 | 95.13 | 5.70 |
Dimethoate | 113.33 | 3.61 | 86.55 | 2.66 | 108.36 | 2.04 | 114.95 | 3.05 | 84.70 | 5.63 | 104.82 | 6.11 |
Diuron | 92.50 | 3.95 | 94.03 | 3.92 | 98.66 | 3.05 | 89.66 | 9.06 | 95.48 | 6.49 | 96.70 | 5.16 |
Fenbuconazole | 109.39 | 2.92 | 99.23 | 6.03 | 99.43 | 3.15 | 102.96 | 6.34 | 99.92 | 6.59 | 95.30 | 5.30 |
Fenoxycarb | 77.40 | 5.05 | 97.15 | 4.95 | 94.10 | 3.31 | 77.08 | 4.39 | 94.05 | 6.04 | 90.84 | 5.43 |
Florasulam | 99.41 | 7.49 | 96.36 | 11.51 | 106.93 | 3.03 | 105.11 | 4.41 | 97.91 | 8.49 | 105.60 | 5.14 |
Fluquinconazole | 102.39 | 13.93 | 86.26 | 8.26 | 89.72 | 3.60 | 91.62 | 16.12 | 88.58 | 7.86 | 85.48 | 5.51 |
Iodosulfuron methyl | 81.15 | 9.06 | 112.43 | 5.97 | 106.61 | 6.18 | 76.96 | 9.89 | 119.75 | 3.51 | 101.11 | 1.62 |
Imazalil | 103.04 | 2.44 | 104.00 | 4.13 | 104.95 | 1.59 | 101.98 | 2.29 | 101.33 | 4.81 | 103.56 | 4.20 |
Deltamethin | 70.58 | 8.73 | 69.75 | 1.26 | 67.12 | 9.23 | 71.41 | 10.79 | 70.16 | 6.07 | 66.94 | 18.55 |
Trifloxystrobin | 96.37 | 2.66 | 109.33 | 4.18 | 95.16 | 3.98 | 93.84 | 4.35 | 106.72 | 5.80 | 93.84 | 1.44 |
Isoproturon | 97.77 | 4.27 | 104.54 | 4.21 | 102.66 | 3.14 | 95.53 | 5.96 | 103.73 | 5.32 | 101.82 | 3.14 |
Kresoxim-methyl | 96.94 | 4.65 | 100.82 | 5.61 | 95.47 | 2.41 | 100.03 | 3.92 | 100.02 | 4.68 | 92.02 | 3.57 |
Metalaxyl | 99.19 | 2.27 | 104.92 | 4.20 | 103.66 | 3.87 | 99.77 | 4.40 | 104.72 | 5.70 | 104.03 | 3.12 |
Florasulam | 99.41 | 7.49 | 96.36 | 11.51 | 106.93 | 3.03 | 105.11 | 4.41 | 97.91 | 8.49 | 105.60 | 5.14 |
Myclobutanil | 101.55 | 2.12 | 98.71 | 4.58 | 99.49 | 3.42 | 99.17 | 3.34 | 99.23 | 6.65 | 95.49 | 3.95 |
Mefenpyr-diethyl | 75.22 | 4.13 | 75.11 | 4.38 | 93.11 | 3.46 | 73.88 | 4.66 | 74.90 | 5.07 | 93.22 | 2.96 |
Nicosulfuron | 107.44 | 3.90 | 101.05 | 6.68 | 106.50 | 2.61 | 96.40 | 5.03 | 97.13 | 14.16 | 103.76 | 6.56 |
Pirimicarb | 93.84 | 3.92 | 92.61 | 4.34 | 98.65 | 4.45 | 93.38 | 3.23 | 89.02 | 4.55 | 98.79 | 5.81 |
Penoxsulam | 104.20 | 3.82 | 83.95 | 5.00 | 90.73 | 2.37 | 102.18 | 6.72 | 83.51 | 5.47 | 88.56 | 5.55 |
Phosmet | 112.37 | 2.32 | 92.74 | 1.78 | 99.66 | 1.54 | 110.68 | 4.01 | 93.05 | 4.13 | 97.04 | 5.05 |
Pyriproxyfen | 49.90 | 6.29 | 60.66 | 4.12 | 58.69 | 2.32 | 48.01 | 4.86 | 59.61 | 8.30 | 58.24 | 3.11 |
Pyraclostrobin | 75.95 | 4.30 | 81.66 | 3.25 | 96.44 | 4.31 | 74.34 | 2.04 | 80.38 | 6.91 | 94.67 | 3.48 |
Quizalofop-p-ethyl | 70.88 | 6.50 | 79.90 | 5.52 | 80.55 | 6.42 | 74.03 | 6.66 | 79.36 | 7.41 | 75.43 | 4.67 |
Spinetoram | 100.45 | 2.60 | 92.00 | 7.25 | 101.09 | 2.91 | 100.11 | 5.42 | 92.54 | 8.25 | 96.91 | 2.95 |
Spirotetramat | 95.26 | 6.15 | 104.02 | 3.96 | 103.72 | 3.81 | 86.37 | 4.70 | 104.39 | 7.79 | 103.52 | 4.19 |
Terbuthylazine | 93.89 | 4.32 | 88.09 | 3.82 | 86.30 | 2.79 | 91.50 | 3.58 | 88.93 | 6.27 | 83.60 | 4.29 |
Thiabendazole | 108.68 | 1.55 | 82.92 | 5.28 | 92.18 | 2.90 | 106.87 | 2.28 | 79.41 | 5.79 | 89.49 | 4.41 |
Thiamethoxam | 103.35 | 6.66 | 108.93 | 2.23 | 101.83 | 2.06 | 100.15 | 7.22 | 105.40 | 3.47 | 98.02 | 3.90 |
Tebuconazole | 97.86 | 1.94 | 103.34 | 6.84 | 98.53 | 3.81 | 95.55 | 4.77 | 103.44 | 6.42 | 96.85 | 3.59 |
Thiacloprid | 107.01 | 3.54 | 94.54 | 5.00 | 99.79 | 1.93 | 105.42 | 4.32 | 93.79 | 5.02 | 97.29 | 6.37 |
Tribenuron-methyl | 106.97 | 4.75 | 89.18 | 4.21 | 96.01 | 2.59 | 106.44 | 5.00 | 88.72 | 5.22 | 92.95 | 3.76 |
λ-cyhalothrin | 68.42 | 2.03 | 71.77 | 8.86 | 80.13 | 11.76 | 71.09 | 7.52 | 79.20 | 3.82 | 78.45 | 23.19 |
Pesticides | ΕΜR-Lipid | Z-Sep+ | ||
---|---|---|---|---|
LOQ (μg/kg) | LOD (μg/kg) | LOQ (μg/kg) | LOD (μg/kg) | |
Alachlor | 3.17 | 1.05 | 5.99 | 1.98 |
Azoxystrobin | 2.38 | 0.79 | 3.02 | 1.00 |
Benalaxyl | 2.33 | 0.77 | 3.16 | 1.04 |
Boscalid | 2.79 | 0.92 | 4.65 | 1.53 |
Chlorfenviphos | 4.06 | 1.34 | 5.02 | 1.66 |
Chlorpyrifos | 3.34 | 1.10 | 2.64 | 0.87 |
Diazinon | 2.20 | 0.72 | 4.97 | 1.64 |
Difenoconazole | 4.08 | 1.35 | 3.33 | 1.10 |
Dimethoate | 3.68 | 1.21 | 2.02 | 0.66 |
Diuron | 3.29 | 1.08 | 2.45 | 0.81 |
Fenbuconazole | 2.87 | 0.95 | 6.47 | 2.13 |
Fenoxycarb | 3.52 | 1.16 | 4.93 | 1.63 |
Florasulam | 6.71 | 2.21 | 4.96 | 1.63 |
Fluquinconazole | 7.83 | 2.58 | 6.73 | 2.22 |
Iodosulfuron methyl | 6.61 | 2.18 | 3.97 | 1.31 |
Imazalil | 2.26 | 0.75 | 6.22 | 2.05 |
Deltamethin | 5.55 | 1.83 | 9.92 | 3.27 |
Trifloxystrobin | 2.31 | 0.76 | 4.87 | 1.61 |
Isoproturon | 3.76 | 1.24 | 4.75 | 1.57 |
Kresoxim-methyl | 4.05 | 1.34 | 4.80 | 1.58 |
Metalaxyl | 2.03 | 0.67 | 1.53 | 0.50 |
Myclobutanil | 1.94 | 0.64 | 6.36 | 2.10 |
Mefenpyr-diethyl | 2.79 | 0.92 | 3.87 | 1.28 |
Nicosulfuron | 3.77 | 1.24 | 5.76 | 1.90 |
Pirimicarb | 3.31 | 1.09 | 2.74 | 0.90 |
Penoxsulam | 3.58 | 1.18 | 3.80 | 1.25 |
Phosmet | 2.35 | 0.77 | 2.12 | 0.70 |
Pyriproxyfen | 2.83 | 0.93 | 1.32 | 0.44 |
Pyraclostrobin | 2.94 | 0.97 | 4.83 | 1.59 |
Quizalofop-p-ethyl | 3.99 | 1.31 | 3.50 | 1.16 |
Spinetoram | 2.35 | 0.77 | 1.25 | 0.41 |
Spirotetramat | 5.27 | 1.74 | 6.00 | 1.97 |
Terbuthylazine | 3.65 | 1.20 | 1.42 | 0.47 |
Thiabendazole | 1.32 | 0.44 | 0.98 | 0.32 |
Thiamethoxam | 6.20 | 2.04 | 2.17 | 0.72 |
Tebuconazole | 1.71 | 0.56 | 1.44 | 0.48 |
Thiacloprid | 3.41 | 1.12 | 3.96 | 1.31 |
Tribenuron-methyl | 4.57 | 1.51 | 2.47 | 0.81 |
λ-cyhalothrin | 2.82 | 0.93 | 3.67 | 1.21 |
Z-Sep+ | EMR-Lipid | |||||||
---|---|---|---|---|---|---|---|---|
30 μg/kg | 100 μg/kg | 300 μg/kg | 30 μg/kg | 100 μg/kg | 300 μg/kg | |||
U (%) | HorRat | U (%) | U (%) | U (%) | HorRat | U (%) | U (%) | |
Alachlor | 17.98 (±1.44) | 0.07 | 8.69 (±7.29) | 5.73(±13.42) | 7.69 (±2.41) | 0.26 | 6.29 (±5.68) | 2.65(±7.44) |
Azoxystrobin | 8.38 (±2.27) | 0.25 | 5.78 (±5.71) | 2.74 (±7.38) | 6.16 (±1.80) | 0.19 | 8.34 (±8.98) | 4.20 (±12.74) |
Benalaxyl | 10.85 (±2.35) | 0.26 | 4.85 (±4.46) | 3.71 (±9.15) | 7.80 (±1.73) | 0.19 | 9.82 (±7.66) | 3.02 (±8.00) |
Boscalid | 14.63 (±3.47) | 0.38 | 5.06 (±4.23) | 4.90 (±11.93) | 6.37 (±2.13) | 0.23 | 6.95 (±6.26) | 3.38 (±9.46) |
Chlorfenviphos | 12.50 (±3.81) | 0.41 | 5.88 (±6.42) | 4.95 (±13.78) | 12.46 (±3.04) | 0.33 | 9.36 (±10.38) | 3.14 (±9.45) |
Chlorpyrifos | 8.25 (±1.97) | 0.22 | 8.35 (±4.86) | 3.87 (±8.21) | 9.96 (±2.50) | 0.27 | 13.00 (±8.02) | 5.20 (±10.61) |
Diazinon | 11.74 (±3.78) | 0.41 | 4.29 (±5.27) | 4.60 (±13.35) | 5.03 (±1.67) | 0.18 | 7.97 (±9.88) | 3.00 (±9.40) |
Difenoconazole | 10.95 (±2.48) | 0.27 | 5.60 (±3.94) | 4.79 (±11.76) | 12.51(±3.05) | 0.33 | 7.28 (±6.43) | 3.40 (±10.06) |
Dimethoate | 5.46 (±1.52) | 0.16 | 4.66 (±4.62) | 2.60 (±6.84) | 8.27 (±2.81) | 0.30 | 6.31 (±5.46) | 4.12 (±13.29) |
Diuron | 7.84 (±1.83) | 0.20 | 5.96 (±4.66) | 4.60 (±12.16) | 8.92 (±2.48) | 0.27 | 6.13 (±5.85) | 3.43 (±10.13) |
Fenbuconazole | 20.51 (±4.83) | 0.53 | 6.44 (±5.42) | 5.25 (±12.26) | 6.67 (±2.19) | 0.23 | 5.08 (±5.17) | 3.46 (±10.17) |
Fenoxycarb | 16.42 (±3.67) | 0.40 | 5.81 (±4.80) | 4.49 (±10.12) | 11.32 (±2.63) | 0.29 | 7.36 (±7.29) | 4.28 (±10.46) |
Florasulam | 12.17 (±3.76) | 0.41 | 6.74 (±4.82) | 5.48 (±13.36) | 17.01 (±5.07) | 0.55 | 17.18 (±5.27) | 4.56 (±14.64) |
Fluquinconazole | 19.54 (±5.05) | 0.55 | 5.73 (±4.68) | 4.90 (±12.75) | 13.14 (±4.11) | 0.44 | 11.85 (±10.78) | 8.50 (±11.86) |
Iodosulfuron methyl | 11.20 (±0.79) | 0.08 | 14.18(±3.34) | 4.40 (±9.95) | 20.32 (±4.95) | 0.54 | 11.71 (±10.41) | 4.38 (±13.21) |
Imazalil | 7.01 (±0.78) | 0.07 | 8.98 (±5.15) | 5.68 (±10.57) | 5.55 (±1.71) | 0.18 | 9.91 (±9.53) | 3.78 (±11.91) |
Deltamethin | 11.95 (±3.12) | 0.29 | 10.59 (±5.67) | 7.59 (±8.37) | 19.49 (±4.13) | 0.45 | 5.59 (±3.86) | 4.84 (±8.99) |
Trifloxystrobin | 13.21 (±3.66) | 0.40 | 3.56 (±3.54) | 3.74 (±10.51) | 6.02 (±1.74) | 0.19 | 6.93 (±7.69) | 4.93 (±13.66) |
Isoproturon | 14.13 (±3.56) | 0.39 | 7.14 (±6.08) | 5.67 (±13.31) | 9.68 (±2.84) | 0.31 | 10.0 (±10.50) | 4.33 (±13.61) |
Kresoxim-methyl | 14.68 (±3.59) | 0.39 | 4.66 (±4.23) | 3.39 (±9.71) | 10.53 (±3.06) | 0.33 | 7.25 (±7.15) | 3.39 (±9.36) |
Metalaxyl | 4.11 (±1.15) | 0.12 | 5.93 (±5.89) | 2.91 (±9.10) | 5.16 (±1.54) | 0.17 | 9.29 (±9.75) | 1.84 (±5.88) |
Myclobutanil | 19.59 (±4.76) | 0.52 | 5.04 (±4.36) | 5.39 (±12.65) | 4.82 (±1.47) | 0.16 | 6.67 (±6.70) | 3.46 (±10.49) |
Mefenpyr-diethyl | 9.41 (±2.94) | 0.32 | 4.81 (±5.26) | 4.39 (±11.77) | 9.23 (±2.08) | 0.23 | 9.78 (±7.35) | 3.74 (±10.54) |
Nicosulfuron | 15.65 (±4.33) | 0.47 | 15.93 (±8.15) | 6.43 (±10.47) | 8.90 (±2.87) | 0.31 | 10.43 (±10.98) | 3.59 (±11.50) |
Pirimicarb | 8.52 (±2.05) | 0.22 | 8.72 (±7.58) | 2.95 (±8.96) | 8.86 (±2.49) | 0.27 | 6.16 (±5.80) | 4.63 (±14.08) |
Penoxsulam | 11.55 (±2.84) | 0.31 | 7.30 (±4.97) | 5.30 (±11.32) | 8.69 (±2.72) | 0.29 | 10.41 (±8.62) | 4.96 (±13.60) |
Phosmet | 5.92 (±1.59) | 0.17 | 3.91 (±3.52) | 3.32 (±9.92) | 5.32 (±1.79) | 0.19 | 4.19 (±3.89) | 3.71 (±11.10) |
Pyriproxyfen | 8.00 (±0.97) | 0.11 | 5.43 (±2.82) | 5.02 (±8.98) | 13.91 (±2.08) | 0.23 | 9.03 (±5.48) | 5.42 (±9.54) |
Pyraclostrobin | 13.51 (±3.63) | 0.39 | 4.09 (±3.96) | 4.34 (±11.03) | 9.62 (±2.19) | 0.24 | 7.38 (±6.02) | 4.91 (±12.54) |
Quizalofop-p-ethyl | 13.94 (±2.59) | 0.29 | 5.53 (±3.99) | 2.51 (±6.73) | 13.94 (±2.96) | 0.33 | 5.23 (±4.08) | 2.76 (±6.55) |
Spinetoram | 15.71 (±0.91) | 0.10 | 26.38 (±3.22) | 23.59 (±14.0) | 5.90 (±1.78) | 0.19 | 5.90 (±5.60) | 3.00 (±9.01) |
Spirotetramat | 16.87 (±4.50) | 0.49 | 6.94 (±6.33) | 4.29 (±12.96) | 13.92 (±3.98) | 0.43 | 9.34 (±9.72) | 4.47 (±13.94) |
Terbuthylazine | 4.81 (±1.06) | 0.12 | 4.73 (±3.70) | 3.72 (±7.97) | 9.76 (±2.75) | 0.30 | 4.78 (±4.28) | 4.33 (±11.18) |
Thiabendazole | 12.88 (±2.73) | 0.08 | 5.66 (±3.27) | 4.76 (±10.95) | 3.09 (±1.00) | 0.11 | 6.56 (±6.05) | 5.63 (±12.14) |
Thiamethoxam | 5.33 (±1.65) | 0.18 | 5.78 (±5.17) | 3.04 (±7.42) | 15.16 (±4.70) | 0.51 | 6.45 (±7.02) | 4.79 (±14.51) |
Tebuconazole | 15.91 (±3.30) | 0.12 | 13.20 (±8.41) | 3.40 (±8.69) | 4.40 (±1.29) | 0.14 | 8.39 (±8.79) | 2.88 (±8.74) |
Thiacloprid | 10.51 (±2.99) | 0.32 | 8.24 (±8.27) | 3.52 (±9.16) | 8.07 (±2.59) | 0.28 | 10.24 (±9.82) | 4.78 (±14.32) |
Tribenuron-methyl | 7.47 (±1.84) | 0.20 | 3.40 (±2.91) | 2.83 (±8.03) | 10.84 (±3.48) | 0.37 | 5.75 (±5.21) | 3.94 (±11.15) |
λ-cyhalothrin | 9.25 (±2.81) | 0.30 | 10.43 (±7.06) | 6.22 (±9.32) | 10.53 (±2.10) | 0.23 | 13.16 (±8.74) | 6.32 (±13.87) |
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Iosif, K.; Konstantinou, I. Determination of Pesticide Residues in Olive Oil Using QuEChERS Extraction and Liquid Chromatography–Orbitrap High-Resolution Mass Spectrometry: Comparison of Different Clean-Up Sorbents and Validation Study. Sustainability 2023, 15, 8714. https://doi.org/10.3390/su15118714
Iosif K, Konstantinou I. Determination of Pesticide Residues in Olive Oil Using QuEChERS Extraction and Liquid Chromatography–Orbitrap High-Resolution Mass Spectrometry: Comparison of Different Clean-Up Sorbents and Validation Study. Sustainability. 2023; 15(11):8714. https://doi.org/10.3390/su15118714
Chicago/Turabian StyleIosif, Konstantina, and Ioannis Konstantinou. 2023. "Determination of Pesticide Residues in Olive Oil Using QuEChERS Extraction and Liquid Chromatography–Orbitrap High-Resolution Mass Spectrometry: Comparison of Different Clean-Up Sorbents and Validation Study" Sustainability 15, no. 11: 8714. https://doi.org/10.3390/su15118714