Determination of Colistin B in Chicken Muscle and Egg Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals, Reagents and Apparatus
2.2. LC–MS/MS Analysis
2.3. Sample Preparation
2.4. Method Validation
3. Results and Discussion
3.1. LC–MS/MS Analysis
3.2. Sample Preparation
3.3. Method Validation
3.3.1. Linearity
3.3.2. Limit of Quantitation (LOQ)
3.3.3. Matrix Effect
3.3.4. Recovery and Precision
3.4. Analysis of Real Samples
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Acknowledgments
Conflicts of Interest
References
- Kumar, H.; Chen, B.H.; Kuca, K.; Nepovimova, E.; Kaushal, A.; Nagraik, R.; Bhatia, S.K.; Dhanjal, D.S.; Kumar, V.; Kumar, A.; et al. Understanding of colistin usage in food animals and available detection techniques: A review. Animals 2020, 10, 1892. [Google Scholar] [CrossRef] [PubMed]
- Bladek, T.; Szymanek, B.I.; Posyniak, A. Determination of polypeptide antibiotic residues in food of animal origin by ultra-high-performance liquid chromatography-tandem mass spectrometry. Molecules 2020, 25, 3261. [Google Scholar] [CrossRef] [PubMed]
- Catry, B.; Cavaleri, M.; Baptiste, K.; Grave, K.; Grein, K.; Holm, A.; Jukes, H.; Liebana, E.; Lopez Navas, A.; Mackay, D.; et al. Use of colistin-containing products within the European Union and European Economic Area (EU/EEA): Development of resistance in animals and possible impact on human and animal health. Int. J. Antimicrob. Agents 2015, 46, 297–306. [Google Scholar] [CrossRef] [PubMed]
- Liu, Y.Y.; Wang, Y.; Walsh, T.R.; Yi, L.X.; Zhang, R.; Spencer, J.; Doi, Y.; Tian, G.; Dong, B.; Huang, X.; et al. Emergence of plasmid-mediated colistin resistance mechanism mcr-1 in animals and human beings in China: A microbiological and molecular biological study. Lancet Infect. Dis. 2016, 16, 161–168. [Google Scholar] [CrossRef]
- Davies, M.; Walsh, T.R. A colistin crisis in India. Lancet Infect. Dis. 2018, 18, 256–257. [Google Scholar] [CrossRef]
- Livemint. Govt May Ban Antibiotic Colistin Used to Fatten Chicken. Available online: https://www.livemint.com/Industry/yt5eE5hqMLYP1px2d63Q1K/Govt-may-ban-antibiotic-colistin-used-to-fatten-chicken.html (accessed on 20 June 2019).
- TOI. Tolerance Limits’ to Be Fixed by Food Regulator for Presence of Antibiotics in Animal, Foods. Available online: https://www.fssai.gov.in/upload/media/FSSAI_News_AntiBiotics_TOI_01_08_2018.pdf (accessed on 12 June 2019).
- FSSAI. Direction under Section 16(5)Read with 18(2)(d)of Food Safety and Standard Act, 2006 Regarding Operationalisation of Draft Food Safety and Standard (Contaminants, Toxins and Residues) Amendment Regulations. 2019. Available online: https://www.fssai.gov.in/upload/advisories/2019/08/5d4c042779d77Direction_Colistin_Ban_FSSAI_08_08_2019.pdf (accessed on 8 September 2019).
- Sin, D.W.; Ho, C.; Wong, Y.C.; Ho, S.K.; Ip, A.C.B. Analysis of major components of residual bacitracin and colistin in food samples by liquid chromatography tandem mass spectrometry. Anal. Chim. Acta 2005, 535, 23–31. [Google Scholar] [CrossRef]
- Wan, E.C.; Ho, C.; Sin, D.W.; Wong, Y.C. Detection of residual bacitracin A, colistin A, and colistin B in milk and animal tissues by liquid chromatography tandem mass spectrometry. Anal. Bioanal. Chem. 2006, 385, 181–188. [Google Scholar] [CrossRef] [PubMed]
- Xu, I.; Tian, X.; Ren, C.; Huang, H.; Zhang, X.; Gong, X.; Liu, H.; Yu, Z.; Zhang, L. Analysis of colistin A and B in fishery products by ultra performance liquid chromatography with positive electro spray ionization tandem mass spectrometry. J. Chromatogr. B 2012, 899, 14–20. [Google Scholar] [CrossRef] [PubMed]
- Boison, J.O.; Lee, S.; Matus, J. A multi-residue method for the determination of seven polypeptide drug residues in chicken muscle tissues by LC-MS/MS. Anal. Bioanal. Chem. 2015, 406, 4065–4078. [Google Scholar] [CrossRef] [PubMed]
- Pascale, R.; Bianco, G.; Coviello, D.; Lafiosca, M.C.; Masi, S.; Mancini, I.M.; Bufo, S.A.; Scrano, L.; Caniani, D. Validation of a LC-MS/MS method for the determination of drugs in wastewater using a three-phase solvent system. J. Sep. Sci. 2020, 43, 886–895. [Google Scholar] [CrossRef] [PubMed]
- SANTE. Available online: https://ec.europa.eu/food/sites/food/files/plant/docs/pesticides_mrl_guidelines_wrkdoc_2019-12682.pdf (accessed on 8 December 2020).
- European Communities. Commission Decision (2002/657/EC) of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off. J. Eur. Communities 2002, L221, 8–36. [Google Scholar]
- Fu, Q.; Li, X.; Zheng, K.; Ke, Y.; Wang, Y.; Wang, L.; Yu, F.; Xia, X. Determination of colistin in animal tissues, egg, milk, and feed by ultra-high performance liquid chromatography-tandem mass spectrometry. Food Chem. 2018, 248, 166–172. [Google Scholar] [CrossRef] [PubMed]
- Saluti, G.; Diamanti, I.; Giusepponi, D.; Pucciarini, L.; Rossi, R.; Moretti, S.; Sardella, R.; Galarini, R. Simultaneous determination of aminoglycosides and colistins in food. Food Chem. 2018, 266, 9–16. [Google Scholar] [CrossRef] [PubMed]
- QuPPe-Method. Available online: https://www.eurl-pesticides.eu/userfiles/file/EurlSRM/meth_QuPPe_AO.pdf (accessed on 10 December 2020).
Target Tissue | MRLs (µg Kg−1) | Regulatory Agency |
---|---|---|
Muscle, Egg | 150, 300 | EU |
Muscle, Egg | 150, 300 | FSSAI |
Muscle | 150 | MAC |
Muscle | 150 | PHR Hong Kong |
Adduct | Precursor ion (m/z) | Product ions (m/z) | RF Lens (V) | CE (eV) | Calibration Range | Linearity | LOQ (µg Kg−1) | % Recovery (RSD %) | ||
---|---|---|---|---|---|---|---|---|---|---|
Muscle | 10 µg Kg−1 | 50 µg Kg−1 | 100 µg Kg−1 | |||||||
[M + 3H]3+ | 386.1 | 374.3 | 122 | 12.12 | 1–50 ng mL−1 | 0.998 | 10 | 71.1 (12.1) | 70.7 (6.6) | 93.8 (3.3) |
[M + 3H]3+ | 386.1 | 380.1 | 10.52 | |||||||
[M + 3H]3+ | 386.1 | 227.1 | 15.83 | |||||||
[M + 3H]3+ | 386.1 | 101.1 | 15.98 | |||||||
Egg | 5 µg Kg−1 | 10 µg Kg−1 | 150 µg Kg−1 | |||||||
[M + 3H]3+ | 386.1 | 374.3 | 122 | 12.12 | 1–25 ng mL−1 | 0.994 | 5 | 88.6 (18.6) | 107.5 (11.5) | 105.5 (2.5) |
[M + 3H]3+ | 386.1 | 380.1 | 10.52 | |||||||
[M + 3H]3+ | 386.1 | 227.1 | 15.83 | |||||||
[M + 3H]3+ | 386.1 | 101.1 | 15.98 |
Sample Type | Sample Weight (g) | Extraction | Clean Up | Evaporation Used | LOQ (µg Kg−1) | References |
---|---|---|---|---|---|---|
Muscle, Egg | 2 | Acetonitrile, Water and Ammonia | NA | Nitrogen | 10 | [2] |
Bovine Liver, Kidney | 0.5 | Trichloroacetic Acid, Acetonitrile, and Formic Acid | OASIS® HLB Sep-pak | Nitrogen | 50 | [9] |
Bovine Muscle, Liver | 2.5 | Hydrochloric Acid | Phenomenex Strata-X cartridges | Nitrogen | 2/5 (MRL) | [10] |
Fishes | 5 | Methanol, Water, and Hydrochloric Acid | ProElut PLS | Nitrogen | 40 | [11] |
Chicken Muscle | 5 | Trichloroacetic Acid, Methanol, Water and Hydrochloric Acid | IRIS Polymeric | Nitrogen | 50 | [12] |
Porcine Muscle, Liver, Kidney; Bovine Muscle, Liver, Kidney; Chicken Muscle, Liver, Kidney, Egg; Sheep Muscle | 2 | Trichloroacetic Acid, and Acetonitrile | Oasis WCX | Nitrogen | 5–30 | [16] |
Bovine Muscle | 3 | Ammonium Acetate, EDTA, Trichloroacetic Acid and Sodium Chloride | Sep-PAK WCX | NA | 33 | [17] |
Chicken Muscle, Egg | 3 | Methanol, Water and Formic Acid | NA | NA | 10 and 5 | Present Study |
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Kumar, H.; Kumar, D.; Nepovimova, E.; Oulkar, D.; Kumar, A.; Azad, R.M.R.; Budakoti, S.K.; Upadhyay, N.K.; Verma, R.; Kuča, K. Determination of Colistin B in Chicken Muscle and Egg Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry. Int. J. Environ. Res. Public Health 2021, 18, 2651. https://doi.org/10.3390/ijerph18052651
Kumar H, Kumar D, Nepovimova E, Oulkar D, Kumar A, Azad RMR, Budakoti SK, Upadhyay NK, Verma R, Kuča K. Determination of Colistin B in Chicken Muscle and Egg Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry. International Journal of Environmental Research and Public Health. 2021; 18(5):2651. https://doi.org/10.3390/ijerph18052651
Chicago/Turabian StyleKumar, Harsh, Dinesh Kumar, Eugenie Nepovimova, Dasharath Oulkar, Anil Kumar, Ramiz Mohammad Rafi Azad, Subodh Kumar Budakoti, Navneet Kumar Upadhyay, Rachna Verma, and Kamil Kuča. 2021. "Determination of Colistin B in Chicken Muscle and Egg Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry" International Journal of Environmental Research and Public Health 18, no. 5: 2651. https://doi.org/10.3390/ijerph18052651