Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. Development of UAE Procedure and Cleanup
2.2. Analytical Evaluation of the Method
2.3. Comparison of the Developed Procedure with Recent UAE-Based Methods in Edible Green Fruits and Leafy Vegetables
2.4. Determination of FQs in Commercial Green Fruits and Leafy Vegetables
3. Materials and Methods
3.1. Chemicals and Materials
3.2. Edible Green Fruits and Leafy Vegetable Samples
3.3. UAE Procedure and Cleanup
3.4. HPLC-ESI-MS/MS
3.5. Analytical Evaluation of the Method
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Analyte | Spinach | Lettuce | Cucumber | ||||||
---|---|---|---|---|---|---|---|---|---|
HQC | MQC | LQC | HQC | MQC | LQC | HQC | MQC | LQC | |
MAR | 92(13) | 91(6) | 92(12) | 91(12) | 96(2) | 92(4) | 105(13) | 86(13) | 106(14) |
NOR | 80(16) | 74(3) | 80(12) | 81(15) | 116(9) | 103(5) | 100(8) | 90(20) | 114(4) |
LEV | 84(9) | 84(16) | 96(10) | 90(3) | 106(5) | 93(16) | 97(8) | 88(11) | 107(4) |
CIP | 75(7) | 81(7) | 91(5) | 80(7) | 88(18) | 90(16) | 89(8) | 83(19) | 111(6) |
DAN | 75(12) | 70(11) | 86(9) | 95(7) | 96(12) | 89(12) | 88(4) | 85(16) | 103(3) |
ENR | 81(10) | 73(8) | 67(6) | 90(2) | 105(3) | 96(9) | 80(15) | 86(15) | 99(4) |
ORB | 80(5) | 95(8) | 81(13) | 89(10) | 93(18) | 94(18) | 84(16) | 75(5) | 100(11) |
Analyte | Spinach | Lettuce | Cucumber | |||
---|---|---|---|---|---|---|
MDL | MQL | MDL | MQL | MDL | MQL | |
MAR | 1 | 4 | 1 | 2 | 2 | 5 |
NOR | 3 | 10 | 2 | 5 | 1 | 3 |
LEV | 2 | 5 | 1 | 2 | 1 | 3 |
CIP | 2 | 5 | 1 | 3 | 2 | 5 |
DAN | 1 | 2 | 1 | 3 | 1 | 2 |
ENR | 1 | 3 | 1 | 2 | 1 | 3 |
ORB | 1 | 3 | 1 | 3 | 1 | 2 |
Matrix | Analyte | UAE | Cleanup | Recovery (%) | MQL (ng g−1) | Ref. |
---|---|---|---|---|---|---|
Cabbage Spinach Radish Corn Rice 1 g (d.w.) | NOR | 3 × 15 min × 30 mL acidified ACN-acetone (1:1 v/v) | HLB™ SPE on 1:200 diluted extract | 81–87 | 1.17 | [18] |
Potato Carrot Lettuce Wheat 250 mg (d.w.) | NOR CIP Ofloxacin | 1 × 5 min × 10 mL ACN−1% CH3COOH (1:1 v/v) | HLB™ SPE on 1:15 diluted extract | 66–93 | 5–40 | [19] |
Lettuce Tomato Cauliflower Bean 1 g (f.w.) | ENR Ofloxacin | 2 × 15 min × 10 mL MeOH | Strata™-X SPE on 1:10 diluted extract | 30–125 | 0.4–9.2 | [9] |
Lettuce 0.2 g (d.w.) | CIP ENR | 2 × 15 min × 5 mL ACN-MeOH−0.5% HCOOH (65:15:20, v/v/v) | C18 d-SPE | 70–90 | 10–24 | [10] |
Spinach Lettuce Cucumber 0.25–0.5 (d.w.) | MAR NOR LEV CIP DAN ENR ORB | 3 × 2 min × 6 mL 20% w/v Mg(NO3)2 2% v/v NH3 | HLB™ SPE on ~1:3 diluted extract | 67–116 | 2–10 | This work |
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Merlo, F.; Centenaro, D.; Maraschi, F.; Profumo, A.; Speltini, A. Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS. Molecules 2022, 27, 6595. https://doi.org/10.3390/molecules27196595
Merlo F, Centenaro D, Maraschi F, Profumo A, Speltini A. Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS. Molecules. 2022; 27(19):6595. https://doi.org/10.3390/molecules27196595
Chicago/Turabian StyleMerlo, Francesca, Dario Centenaro, Federica Maraschi, Antonella Profumo, and Andrea Speltini. 2022. "Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS" Molecules 27, no. 19: 6595. https://doi.org/10.3390/molecules27196595