Simultaneous Determination of Tetracyclines and Fluoroquinolones in Poultry Eggs by UPLC Integrated with Dual-Channel-Fluorescence Detection Method
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Stock and Working Solutions
2.3. UPLC-FLD Analysis
2.4. Sample Collection and Pretreatment
2.5. Method Validation
2.5.1. Linearity
2.5.2. Recovery
2.5.3. Precision
2.5.4. Sensitivity
3. Results and Discussion
3.1. Optimization of the Sample Pretreatment
3.2. Optimization of UPLC Separation and FLD
3.3. Validation
3.4. Applications
3.5. Comparison with Previously Reported Methods
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Matrix | Analyte | Linearity Range (µg/kg) | Linear Regression Equation | Determination Coefficient (R2) |
---|---|---|---|---|
Blended whole chicken egg | OTC | 19.2–1000.0 | y = 425.51x − 2034.3 | 0.9998 |
TC | 31.2–1000.0 | y = 360.26x + 1118.4 | 0.9998 | |
DOX | 35.3–300.0 | y = 248.98x + 7889.8 | 0.9993 | |
CIP | 0.6–300.0 | y = 35325x − 9347 | 0.9998 | |
ENR | 0.4–300.0 | y = 39161x + 282018 | 0.9998 | |
Chicken albumen | OTC | 17.4–1000.0 | y = 418.55x − 1723.3 | 0.9997 |
TC | 28.8–1000.0 | y = 396.38x − 3708.4 | 0.9994 | |
DOX | 31.9–300.0 | y = 281.71x + 3259.9 | 0.9992 | |
CIP | 0.7–300.0 | y = 33285x + 10819 | 0.9996 | |
ENR | 0.3–300.0 | y = 37248x + 398456 | 0.9996 | |
Chicken yolk | OTC | 25.6–1000.0 | y = 449.03x − 6847.2 | 0.9994 |
TC | 36.0–1000.0 | y = 363.79x − 4823.8 | 0.9993 | |
DOX | 40.1–300.0 | y = 286.29x − 71.871 | 0.9998 | |
CIP | 1.2–300.0 | y = 35999x + 30938 | 0.9996 | |
ENR | 0.3–300.0 | y = 43943x + 166512 | 0.9994 | |
Blended whole duck egg | OTC | 20.1–1000.0 | y = 476.11x − 5044.9 | 0.9999 |
TC | 32.1–1000.0 | y = 359.6x + 1599.6 | 0.9998 | |
DOX | 34.7–300.0 | y = 302.9x − 2627.5 | 0.9995 | |
CIP | 1.1–300.0 | y = 36124x − 20065 | 0.9997 | |
ENR | 0.5–300.0 | y = 44043x + 124503 | 0.9997 | |
Duck albumen | OTC | 19.2–1000.0 | y = 444.68x − 968.85 | 0.9996 |
TC | 27.3–1000.0 | y = 394.95x − 7178.2 | 0.9994 | |
DOX | 32.5–300.0 | y = 296.54x − 815.06 | 0.9994 | |
CIP | 0.7–300.0 | y = 35712x + 126377 | 0.9998 | |
ENR | 0.4–300.0 | y = 39981x + 118026 | 0.9995 | |
Duck yolk | OTC | 21.6–1000.0 | y = 413.89x + 538.36 | 0.9997 |
TC | 38.3–1000.0 | y = 333.34x − 3420.4 | 0.9998 | |
DOX | 37.2–300.0 | y = 281.82x + 29.831 | 0.9995 | |
CIP | 1.5–300.0 | y = 40759x + 79433 | 0.9998 | |
ENR | 0.3–300.0 | y = 39750x + 220046 | 0.9993 |
Analyte | Spiked Level (µg/kg) | Recovery (%) | RSD (%) | Intraday RSD (%) | Interday RSD (%) |
---|---|---|---|---|---|
OTC | 19.2 | 86.93 ± 1.39 | 1.60 | 2.59 | 2.78 |
200 | 86.90 ± 2.56 | 2.95 | 3.71 | 3.83 | |
400 α | 89.43 ± 1.63 | 1.82 | 2.03 | 2.32 | |
800 | 91.15 ± 3.21 | 3.52 | 4.52 | 4.72 | |
TC | 31.2 | 86.58 ± 2.88 | 3.32 | 4.14 | 4.26 |
200 | 87.40 ± 1.70 | 1.95 | 3.85 | 3.57 | |
400 α | 89.28 ± 2.48 | 2.78 | 2.85 | 3.89 | |
800 | 90.20 ± 1.38 | 1.53 | 2.33 | 2.58 | |
DOX | 35.3 | 86.33 ± 2.25 | 2.60 | 3.61 | 3.13 |
50 | 85.10 ± 3.01 | 3.54 | 3.10 | 3.94 | |
100 α | 85.15 ± 1.87 | 2.19 | 3.17 | 3.70 | |
200 | 84.65 ± 3.72 | 4.40 | 3.98 | 4.59 | |
CIP | 0.6 | 87.65 ± 2.29 | 2.60 | 3.49 | 3.90 |
50 | 89.88 ± 2.23 | 2.48 | 3.62 | 3.41 | |
100 α | 92.35 ± 2.16 | 2.34 | 2.46 | 3.99 | |
200 | 92.88 ± 2.41 | 2.60 | 2.05 | 3.27 | |
ENR | 0.4 | 94.05 ± 1.88 | 1.99 | 3.07 | 4.17 |
50 | 88.63 ± 2.49 | 2.80 | 2.93 | 3.61 | |
100 α | 95.58 ± 3.68 | 3.85 | 3.41 | 3.90 | |
200 | 92.63 ± 2.57 | 2.78 | 3.15 | 3.74 |
Analyte | Spiked Level (µg/kg) | Recovery (%) | RSD (%) | Intraday RSD (%) | Interday RSD (%) |
---|---|---|---|---|---|
OTC | 17.4 | 87.28 ± 1.76 | 2.01 | 2.57 | 3.96 |
200 | 86.33 ± 1.07 | 1.24 | 2.04 | 2.86 | |
400 α | 89.70 ± 2.60 | 2.90 | 3.15 | 3.09 | |
800 | 89.03 ± 3.30 | 3.71 | 4.28 | 4.32 | |
TC | 28.8 | 85.60 ± 3.15 | 3.69 | 3.82 | 3.95 |
200 | 85.20 ± 1.53 | 1.79 | 2.24 | 3.40 | |
400 α | 90.05 ± 3.40 | 3.77 | 2.68 | 4.84 | |
800 | 89.28 ± 2.42 | 2.70 | 2.67 | 3.64 | |
DOX | 31.9 | 86.20 ± 2.15 | 2.50 | 3.41 | 3.57 |
50 | 86.40 ± 1.54 | 1.79 | 2.23 | 2.37 | |
100 α | 87.53 ± 2.00 | 2.29 | 2.99 | 3.07 | |
200 | 89.58 ± 1.67 | 1.86 | 2.13 | 2.44 | |
CIP | 0.7 | 88.45 ± 2.65 | 2.99 | 2.59 | 3.69 |
50 | 88.13 ± 1.72 | 1.96 | 2.32 | 2.66 | |
100 α | 90.15 ± 1.22 | 1.35 | 1.99 | 2.10 | |
200 | 90.78 ± 1.96 | 2.16 | 2.69 | 2.54 | |
ENR | 0.3 | 86.15 ± 3.52 | 4.09 | 4.67 | 6.24 |
50 | 91.48 ± 1.78 | 1.94 | 2.36 | 4.18 | |
100 α | 89.58 ± 1.51 | 1.69 | 2.65 | 2.81 | |
200 | 91.45 ± 3.36 | 3.67 | 4.31 | 4.94 |
Analyte | Spiked Level (µg/kg) | Recovery (%) | RSD (%) | Intraday RSD (%) | Interday RSD (%) |
---|---|---|---|---|---|
OTC | 25.6 | 85.30 ± 2.17 | 2.54 | 2.95 | 4.10 |
200 | 86.53 ± 1.35 | 1.56 | 3.62 | 3.91 | |
400 α | 87.93 ± 2.40 | 2.73 | 2.94 | 4.92 | |
800 | 88.85 ± 2.96 | 3.33 | 3.35 | 4.12 | |
TC | 36.0 | 86.58 ± 2.88 | 3.32 | 3.55 | 3.97 |
200 | 86.70 ± 1.16 | 1.34 | 3.29 | 3.11 | |
400 α | 88.05 ± 2.00 | 2.27 | 2.56 | 3.99 | |
800 | 89.15 ± 1.07 | 1.20 | 2.77 | 3.63 | |
DOX | 40.1 | 86.08 ± 1.83 | 2.12 | 2.35 | 3.97 |
50 | 86.03 ± 2.70 | 3.15 | 3.63 | 4.71 | |
100 α | 85.15 ± 1.87 | 2.20 | 3.17 | 3.77 | |
200 | 85.13 ± 2.79 | 3.28 | 3.89 | 4.28 | |
CIP | 1.2 | 87.38 ± 1.89 | 2.17 | 2.38 | 3.89 |
50 | 89.63 ± 1.99 | 2.22 | 3.03 | 3.82 | |
100 α | 91.85 ± 2.45 | 2.66 | 3.19 | 3.66 | |
200 | 92.88 ± 2.41 | 2.60 | 3.05 | 3.27 | |
ENR | 0.3 | 90.73 ± 1.70 | 1.88 | 2.07 | 3.37 |
50 | 90.38 ± 2.00 | 2.20 | 2.74 | 3.30 | |
100 α | 95.58 ± 3.68 | 3.85 | 4.11 | 5.60 | |
200 | 93.88 ± 2.66 | 2.83 | 3.31 | 3.45 |
Analyte | Spiked Level (µg/kg) | Recovery (%) | RSD (%) | Intraday RSD (%) | Interday RSD (%) |
---|---|---|---|---|---|
OTC | 20.1 | 85.33 ± 2.87 | 3.36 | 3.50 | 4.55 |
200 | 85.78 ± 1.60 | 1.86 | 2.66 | 3.30 | |
400 α | 88.38 ± 1.88 | 2.13 | 2.91 | 3.11 | |
800 | 89.40 ± 2.50 | 2.81 | 3.85 | 4.19 | |
TC | 32.1 | 87.30 ± 2.15 | 2.46 | 3.61 | 4.48 |
200 | 87.58 ± 2.18 | 2.49 | 3.20 | 3.55 | |
400 α | 88.35 ± 2.50 | 2.83 | 3.38 | 3.40 | |
800 | 89.18 ± 1.72 | 1.93 | 2.57 | 3.14 | |
DOX | 34.7 | 84.33 ± 2.68 | 3.18 | 3.62 | 4.51 |
50 | 83.50 ± 1.10 | 1.32 | 3.12 | 3.31 | |
100 α | 86.15 ± 3.33 | 3.87 | 3.22 | 4.28 | |
200 | 84.83 ± 1.26 | 1.49 | 3.58 | 3.46 | |
CIP | 1.1 | 85.53 ± 2.05 | 2.40 | 3.51 | 4.17 |
50 | 90.13 ± 2.66 | 2.95 | 3.68 | 4.14 | |
100 α | 91.80 ± 1.94 | 2.11 | 2.91 | 3.39 | |
200 | 92.03 ± 2.96 | 3.21 | 3.60 | 4.45 | |
ENR | 0.5 | 87.98 ± 3.12 | 3.55 | 3.46 | 4.01 |
50 | 89.13 ± 2.65 | 2.97 | 3.29 | 3.04 | |
100 α | 94.35 ± 2.80 | 2.97 | 3.93 | 4.30 | |
200 | 92.63 ± 2.57 | 2.78 | 2.11 | 3.24 |
Analyte | Spiked Level (µg/kg) | Recovery (%) | RSD (%) | Intraday RSD (%) | Interday RSD (%) |
---|---|---|---|---|---|
OTC | 19.2 | 87.03 ± 2.14 | 2.46 | 3.57 | 4.22 |
200 | 87.58 ± 1.82 | 2.08 | 3.83 | 3.54 | |
400 α | 88.48 ± 2.11 | 2.39 | 2.80 | 3.12 | |
800 | 88.18 ± 2.20 | 2.49 | 3.03 | 4.96 | |
TC | 27.3 | 84.10 ± 3.50 | 4.17 | 4.91 | 5.55 |
200 | 86.33 ± 2.91 | 3.37 | 4.25 | 4.68 | |
400 α | 88.90 ± 3.66 | 4.12 | 4.06 | 5.28 | |
800 | 89.23 ± 2.12 | 2.38 | 3.86 | 3.37 | |
DOX | 32.5 | 84.45 ± 2.18 | 2.58 | 3.51 | 4.78 |
50 | 85.88 ± 1.52 | 1.77 | 2.35 | 3.17 | |
100 α | 86.68 ± 3.40 | 3.92 | 3.96 | 5.80 | |
200 | 88.88 ± 1.79 | 2.02 | 3.76 | 3.69 | |
CIP | 0.7 | 88.45 ± 2.65 | 2.99 | 3.55 | 4.11 |
50 | 87.85 ± 1.22 | 1.39 | 3.32 | 3.16 | |
100 α | 88.90 ± 3.53 | 3.98 | 4.70 | 5.33 | |
200 | 89.08 ± 1.60 | 1.79 | 2.07 | 3.88 | |
ENR | 0.4 | 87.90 ± 3.26 | 3.70 | 3.95 | 4.42 |
50 | 90.98 ± 1.71 | 1.88 | 3.20 | 3.23 | |
100 α | 89.85 ± 2.05 | 2.28 | 3.23 | 4.77 | |
200 | 91.23 ± 3.50 | 3.84 | 2.88 | 4.27 |
Analyte | Spiked Level (µg/kg) | Recovery (%) | RSD (%) | Intraday RSD (%) | Interday RSD (%) |
---|---|---|---|---|---|
OTC | 21.6 | 86.93 ± 1.39 | 1.60 | 3.54 | 3.59 |
200 | 86.85 ± 2.56 | 2.95 | 3.71 | 4.83 | |
400 α | 89.43 ± 1.63 | 1.82 | 2.13 | 3.32 | |
800 | 91.15 ± 3.21 | 3.52 | 3.86 | 4.72 | |
TC | 38.3 | 86.58 ± 2.88 | 3.32 | 3.14 | 4.26 |
200 | 87.40 ± 1.70 | 1.95 | 2.95 | 2.57 | |
400 α | 89.28 ± 2.48 | 2.78 | 2.87 | 3.26 | |
800 | 90.20 ± 1.38 | 1.53 | 3.58 | 3.33 | |
DOX | 37.2 | 86.33 ± 2.25 | 2.60 | 3.25 | 4.13 |
50 | 85.10 ± 3.01 | 3.54 | 3.48 | 5.10 | |
100 α | 87.65 ± 1.60 | 1.84 | 2.37 | 3.19 | |
200 | 90.90 ± 2.40 | 2.64 | 3.66 | 3.23 | |
CIP | 1.5 | 88.65 ± 3.30 | 3.72 | 4.11 | 4.52 |
50 | 89.88 ± 2.23 | 2.48 | 2.62 | 3.41 | |
100 α | 92.35 ± 2.16 | 2.34 | 3.46 | 3.99 | |
200 | 92.63 ± 2.03 | 2.19 | 3.09 | 4.53 | |
ENR | 0.3 | 89.73 ± 1.42 | 1.59 | 2.40 | 3.66 |
50 | 90.48 ± 1.60 | 1.78 | 2.82 | 3.86 | |
100 α | 92.51 ± 3.68 | 3.98 | 3.11 | 4.26 | |
200 | 92.63 ± 2.57 | 2.78 | 3.17 | 3.24 |
Analyte | Matrix | LODs (µg/kg) | LOQs (µg/kg) |
---|---|---|---|
OTC | Blended whole chicken egg | 5.5 | 19.2 |
Chicken albumen | 5.2 | 17.4 | |
Chicken Yolk | 7.7 | 25.6 | |
Blended whole duck egg | 6.0 | 20.1 | |
Duck albumen | 5.4 | 19.2 | |
Duck yolk | 6.5 | 21.6 | |
TC | Blended whole chicken egg | 9.1 | 31.2 |
Chicken albumen | 9.5 | 28.8 | |
Chicken yolk | 10.6 | 36.0 | |
Blended whole duck egg | 9.3 | 32.1 | |
Duck albumen | 8.9 | 27.3 | |
Duck yolk | 11.8 | 38.3 | |
DOX | Blended whole chicken egg | 10.5 | 35.3 |
Chicken albumen | 9.7 | 31.9 | |
Chicken yolk | 13.4 | 40.1 | |
Blended whole duck egg | 10.4 | 34.7 | |
Duck albumen | 9.6 | 32.5 | |
Duck yolk | 10.6 | 37.2 | |
CIP | Blended whole chicken egg | 0.2 | 0.6 |
Chicken albumen | 0.2 | 0.7 | |
Chicken yolk | 0.4 | 1.2 | |
Blended whole duck egg | 0.3 | 1.1 | |
Duck albumen | 0.2 | 0.7 | |
Duck yolk | 0.5 | 1.5 | |
ENR | Blended whole chicken egg | 0.1 | 0.4 |
Chicken albumen | 0.1 | 0.3 | |
Chicken yolk | 0.1 | 0.3 | |
Blended whole duck egg | 0.1 | 0.5 | |
Duck albumen | 0.1 | 0.4 | |
Duck yolk | 0.1 | 0.3 |
Detection Method | Sample Pretreatment Method | Analyte | Matrix | Analysis Time (min) | LOD (µg/kg) | LOQ (µg/kg) | Recovery (%) |
---|---|---|---|---|---|---|---|
UPLC-FLD (this study) | LLE-SPE | Tetracyclines and fluoroquinolones | Poultry eggs | 9 | 0.1–13.4 | 0.3–40.1 | 83.50–95.58 |
UPLC-FLD [10] | Dispersive SPE | Tetracyclines and acidic quinolones | Pork and chicken muscle | 6 | 0.25–3.8 | - | 61.5–102.6 |
HPLC-FLD [19] | LLE | Tetracyclines and fluoroquinolones | Catfish muscle | >25 | - | 0.15–1.5 | 60–92 |
HPLC-FLD [20] | LLE | Tetracyclines and fluoroquinolones | Chicken muscle | >25 | - | 0.5–5 | 63–95 |
UPLC-DAD [28] | Matrix solid-phase dispersion | Tetracyclines, fluoroquinolones and sulfonamides | Pork | 14 | 0.5–3.0 | - | 74.5–102.7 |
HPLC-DAD [29] | Matrix solid-phase dispersion | Tetracyclines and fluoroquinolones | Porcine tissues | 12 | 2–10 | 7–34 | 80.6–99.2 |
HPLC-DAD [21] | LLE-SPE | Tetracyclines, fluoroquinolones, sulfonamides and chloramphenicols | Milk | 40 | 17.2–24.9 | 51.5–68.1 | 83.3–111.8 |
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Guo, Y.; He, Z.; Chen, J.; Chen, L.; Xie, K.; Zhang, T.; Zhang, G.; Dai, G. Simultaneous Determination of Tetracyclines and Fluoroquinolones in Poultry Eggs by UPLC Integrated with Dual-Channel-Fluorescence Detection Method. Molecules 2021, 26, 5684. https://doi.org/10.3390/molecules26185684
Guo Y, He Z, Chen J, Chen L, Xie K, Zhang T, Zhang G, Dai G. Simultaneous Determination of Tetracyclines and Fluoroquinolones in Poultry Eggs by UPLC Integrated with Dual-Channel-Fluorescence Detection Method. Molecules. 2021; 26(18):5684. https://doi.org/10.3390/molecules26185684
Chicago/Turabian StyleGuo, Yawen, Zhaoyuan He, Jinyuan Chen, Lan Chen, Kaizhou Xie, Tao Zhang, Genxi Zhang, and Guojun Dai. 2021. "Simultaneous Determination of Tetracyclines and Fluoroquinolones in Poultry Eggs by UPLC Integrated with Dual-Channel-Fluorescence Detection Method" Molecules 26, no. 18: 5684. https://doi.org/10.3390/molecules26185684