Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography–Tandem Mass Spectrometry
Abstract
:1. Introduction
2. Results and Discussion
2.1. HPLC–MS/MS Conditions
2.2. Method Development
2.3. Method Validation
2.4. Application of the Method
3. Materials and Methods
3.1. Materials
3.2. Instrumentation and Chromatographic Conditions
3.3. Standard Stock Solutions Preparation
3.4. Method Validation
3.5. Sample Collection and Sample Preparation
3.6. Statistical Analysis
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Compounds | Retention Time (min) | Q1 Mass (m/z) | Q3 Mass (m/z) | Collision Energy (eV) | Ion Ratio (%) |
---|---|---|---|---|---|
MB | 3.48 | 284.0 | 268.1 1/252.0 | 34/49 | 28 |
AZA | 2.49 | 256.1 | 241.0 1/199.0 | 32/33 | 70 |
AZB | 2.98 | 270.1 | 254.1 1/212.0 | 34/51 | 30 |
AZC | 1.84 | 242.1 | 200.1 1/227.0 | 33/26 | 34 |
Compounds | LR (µg/kg) | R2 | LOD (µg/kg) | LOQ (µg/kg) | Intraday RSD (n = 3) (%) | Inter-Day RSD (n = 3, day) (%) | ME (%) |
---|---|---|---|---|---|---|---|
MB | 1–500 | 0.9982 | 0.75 | 1.0 | 4.95 | 6.47 | 2.9 |
AZA | 1–500 | 0.9966 | 0.75 | 1.0 | 6.75 | 8.50 | 12.8 |
AZB | 1–500 | 0.9978 | 0.75 | 1.0 | 4.34 | 5.61 | 7.0 |
AZC | 1–500 | 0.9959 | 0.75 | 1.0 | 7.08 | 9.59 | 15.9 |
Analytes | Add Level(µg/kg) | Recovery/% (RSD/%) | ||||||||
---|---|---|---|---|---|---|---|---|---|---|
Bream | Trout | Grass Carp | Fresh Shrimps | Chinese Mitten Crab | Crucian Carp | Perch | Catfish | Mussel | ||
MB | 1 | 93.2 (2.63) | 96.5 (4.27) | 95.2 (4.51) | 96.7 (7.04) | 89.9 (6.58) | 92.7 (3.04) | 91.5 (2.21) | 90.5 (4.18) | 89.7 (6.24) |
5 | 90.5 (5.23) | 95.0 (4.01) | 93.4 (3.28) | 95.1 (3.24) | 91.1 (5.63) | 93.3 (5.32) | 93.5 (3.08) | 96.0 (5.36) | 90.5 (6.06) | |
10 | 96.4 (6.37) | 95.3 (7.68) | 92.5 (4.05) | 97.5 (2.84) | 90.7 (6.70) | 90.5 (5.01) | 93.9 (4.29) | 93.2 (1.05) | 91.5 (5.71) | |
AZA | 1 | 86.2 (7.15) | 82.9 (7.52) | 88.9 (3.57) | 87.2 (6.35) | 83.2 (8.04) | 86.1 (3.82) | 88.6 (3.66) | 83.5 (6.01) | 81.6 (1.28) |
5 | 88.3 (8.63) | 84.9 (7.67) | 90.7 (3.69) | 84.9 (5.08) | 86.4 (8.36) | 83.1 (3.66) | 87.9 (2.08) | 85.5 (5.47) | 82.0 (1.38) | |
10 | 91.0 (5.72) | 89.5 (5.34) | 91.0 (2.61) | 86.5 (7.04) | 88.7 (6.04) | 88.6 (2.79) | 89.2 (1.99) | 83.9 (3.28) | 85.0 (1.98) | |
AZB | 1 | 95.3 (4.25) | 96.0 (5.05) | 97.1 (1.07) | 95.4 (5.60) | 92.5 (7.74) | 94.3 (1.35) | 92.8 (5.27) | 91.8 (2.04) | 93.4 (3.06) |
5 | 96.0 (3.35) | 94.2 (4.75) | 95.0 (2.67) | 96.2 (5.07) | 93.4 (6.66) | 90.5 (2.07) | 90.8 (3.31) | 93.0 (1.29) | 96.0 (1.08) | |
10 | 94.2 (3.07) | 93.8 (5.01) | 93.8 (1.96) | 93.7 (4.14) | 95.2 (4.24) | 92.0 (1.72) | 95.4 (3.07) | 91.2 (2.22) | 94.4 (1.66) | |
AZC | 1 | 73.2 (3.58) | 75.1 (5.05) | 74.5 (3.77) | 72.1 (5.74) | 71.8 (8.05) | 75.4 (4.76) | 74.8 (6.12) | 75.5 (7.22) | 72.1 (6.01) |
5 | 72.8 (4.57) | 77.0 (5.34) | 74.3 (3.04) | 75.4 (4.87) | 72.2 (6.80) | 73.5 (5.33) | 73.0 (5.76) | 72.0 (2.05) | 74.2 (5.20) | |
10 | 75.7 (3.39) | 78.7 (1.87) | 72.7 (3.30) | 72.7 (5.02) | 78.1 (6.17) | 78.6 (4.21) | 72.8 (3.35) | 74.6 (5.00) | 76.6 (6.45) |
Extraction Organic Solvent | Purification Agent | Sample | N 1 | LR (µg/L) | LOQ (µg/kg) | RSD (%) | Recovery (%) | Ref. |
---|---|---|---|---|---|---|---|---|
Acetonitrile | ALN cartridge | Aquatic products | 4 | 1–500 | 1.0 | 1.05–8.63 | 71.8–97.5 | Present method |
Acetonitrile containing 0.1% of formic acid | - | Aquatic products | 4 | 0.04–2.0 | 0.4–4 | 5–15 | 87–130 | [18] |
Ammonium acetate buffer solution and acetonitrile | Liquid–liquid distribution and PRS 2 cartridge | Aquatic products | 4 | 1–100 | 2 | 2.3–13.0 | 70.3–92.1 | [19] |
Acetonitrile | - | Plasma | 2 | 1–1000 | 30 | 3.6–11.9 | 97.9–108.0 | [20] |
Acetonitrile | CBA and SCX-SPE 3 cartridges | Eel | 2 | 2–16 | 0.25 | 8.3–14.5 | 84.1–102.1 | [21] |
Acetonitrile/sodium acetate buffer solution | ALN cartridge | Eel, toasted eel, and shrimp | 1 | 2.0–100.0 | 0.5 | 4.4–16.3 | 73.0–108.3 | [22] |
Time (min) | Mobile Phase A (%) | Mobile Phase B (%) | Mobile Phase C (%) |
---|---|---|---|
0.0 | 63 | 22 | 15 |
2.4 | 63 | 22 | 15 |
2.5 | 28 | 42 | 30 |
7.0 | 28 | 42 | 30 |
7.1 | 0 | 60 | 40 |
15.0 | 0 | 60 | 40 |
15.1 | 63 | 22 | 15 |
18.0 | 63 | 22 | 15 |
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Zhang, X.; Hui, Y.; Fang, C.; Wang, Y.; Han, F.; Lou, X.; Fodjo, E.K.; Cai, Y.; Kong, C. Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography–Tandem Mass Spectrometry. Molecules 2021, 26, 4975. https://doi.org/10.3390/molecules26164975
Zhang X, Hui Y, Fang C, Wang Y, Han F, Lou X, Fodjo EK, Cai Y, Kong C. Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography–Tandem Mass Spectrometry. Molecules. 2021; 26(16):4975. https://doi.org/10.3390/molecules26164975
Chicago/Turabian StyleZhang, Xuan, Yunhua Hui, Changling Fang, Yuan Wang, Feng Han, Xiaoyi Lou, Essy Kouadio Fodjo, Youqiong Cai, and Cong Kong. 2021. "Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography–Tandem Mass Spectrometry" Molecules 26, no. 16: 4975. https://doi.org/10.3390/molecules26164975