Determination of sulphamethoxazole and carbamazepine in waste and surface water of Shymkent city

Aim. The development of a liquid chromatography method for the quantitative determination of Sulfamethoxazole and Carbamazepine in wastewater from sewage systems and surface waters of the city of Shymkent.

Materials and methods. The chromatographic system DIONEX UltiMate 3000 with diode-array detector at absorption wavelength of 254 nm, reversed-phase version with mobile phase of acetonitrile-water composition (40: 60) and with a Hypersil GOLD C8 150x2.1 mm 1.9 micron column filled with porous ultrapurified silica gel, the thermostat temperature of the chromatographic column was 30 0C. Elution was carried out in isocratic mode. The total analysis time for 1 sample was 30 min. The flow rate of mobile phase was 1 ml/min. The retention time of standard sample solutions of carbamazepine was 3.612±0.1 min, for sulfamethoxazole – 6.910±0.1 min.

Results and discussion. A validated method for the detection and quantification of drug residues in water samples using the UHPLC-DAD method has been developed: the correlation coefficient of the linear regression graph was 0.9999; the relative standard deviation of the method for sulfamethoxazole and carbamazepine between samples within a cycle was 0.08110.7354%, between cycles – 0.1660-1.6457%. Monitoring of drug contamination of the studied waste and surface waters were carried out. At low concentrations, sulfamethoxazole and carbamazepine were detected and quantified in waste and surface waters of the Shymkent city. Under chromatographic conditions, the retention time of carbamazepine was 3.612±0.1 min, of sulfamethoxazole – 6.910±0.1 min, which corresponds to the retention times of the standard sample solutions.

Conclusions. A method for the study of water samples for the content of pharmaceutical residues using HPLC-DAD was developed and validated: the correlation coefficient of the linear regression graph was 0.9999; the relative error for carbamazepine ranged from 0.0166% to 1.6457%, and for sulfamethoxazole from 0.3888% to 0.8212%, confirming the high reproducibility of the developed method, which is suitable for further analytical research.

Based on the results of the study of water samples, the quantitative content of carbamazepine and sulfamethoxazole in wastewater and surface waters of Shymkent was determined during the initial study in the autumn period. The results of preliminary studies form the basis for further research on wastewater and surface waters for the presence of pharmaceutical residues to monitor the ecological situation in the region.

1. Water, sanitation, hygiene, waste and electricity services in health care facilities: progress on the fundamentals. 2023 global report. Geneva: World Health Organization and the United Nations Children’s Fund (UNICEF); 2023: 80.

2. Ending the neglect to attain the Sustainable Development Goals: a global strategy on water, sanitation and hygiene to combat neglected tropical diseases, 2021- 2030. Geneva: World Health Organization and the United Nations Children’s Fund (UNICEF); 2023: 36.

3. «OON-Vodnye resursy», 2021 god: Kratkij obzor Doklada o progresse 2021 goda: CUR 6 — vodosnabzhenie i sanitarija dlja vseh.Versija: ijul’ 2021 goda. Zheneva; 58.

4. Hai F. I. Carbamazepine as a possible anthropogenic marker in water: occurrences, toxicological effects, regulations and removal by wastewater treatment technologies. Water. 2018; 10 (2): 107.

5. Kasprzyk-Hordern B., Dinsdale R.M., Guwy A.J. Illicit drugs and pharmaceuticals in the environment–Forensic applications of environmental data. Part 1: Estimation of the usage of drugs in local communities. Environmental Pollution. 2009; 157 (6): 1773-1777.

6. Singer H. Determination of biocides and pesticides by on-line solid phase extraction coupled with mass spectrometry and their behaviour in wastewater and surface water. Environmental pollution. 2010; 158 (10): 3054-3064.

7. Dvory N. Z. Modeling sewage leakage and transport in carbonate aquifer using carbamazepine as an indicator. Water research. 2018; 128: 157-170.

8. Ying G.G., Kookana R.S., Kolpin D.W. Occurrence and removal of pharmaceutically active compounds in sewage treatment plants with different technologies. Journal of Environmental monitoring. 2009; 11 (8): 1498-1505.

9. Tixier C. Occurrence and fate of carbamazepine, clofibric acid, diclofenac, ibuprofen, ketoprofen, and naproxen in surface waters. Environmental science & technology. 2003; 37 (6): 1061-1068.

10. Wijekoon K. C. The fate of pharmaceuticals, steroid hormones, phytoestrogens, UV-filters and pesticides during MBR treatment. Bioresource technology. 2013; 144: 247-254.

11. Iglesias A. Monitoring the presence of 13 active compounds in surface water collected from rural areas in Northwestern Spain. International journal of environmental research and public health. 2014; 11 (5): 5251-5272.

12. Pastor-Navarro N., Maquieira Á., Puchades R. Review on immunoanalytical determination of tetracycline and sulfonamide residues in edible products. Analytical and bioanalytical chemistry. 2009; 395: 907-920.

13. Kovalakova P., Cizmas L., McDonald T.J., Marsalek B., Feng M., Sharma V.K. Occurrence and toxicity of antibiotics in the aquatic environment: A review. Chemosphere. 2020; 251: 126351. https://doi.org/10.1016/j.chemosphere.2020.126351

14. Lorenzo P., Adriana A., Jessica S., Carles B., Marinella F., Marta L., Luis B.J., Pierre S. Antibiotic resistance in urban and hospital wastewaters and their impact on a receiving freshwater ecosystem. Chemosphere. 2018; 206: 70-82. https://doi.org/10.1016/j.chemosphere.2018.04.163

15. Ngigi A.N., Magu M.M., Muendo B.M. Occurrence of antibiotics residues in hospital wastewater, wastewater treatment plant, and in surface water in Nairobi County, Kenya. Environ. Monit. Assess. 2019; 192 (1): 18. https://doi.org/10.1007/s10661-019-7952-8

16. Nantaba F., Wasswa J., Kylin H., Palm W.U., Bouwman H., Kümmerer K. Occurrence, distribution, and ecotoxicological risk assessment of selected pharmaceutical compounds in water from Lake Victoria, Uganda. Chemosphere. 2020; 239: 124642. https://doi.org/10.1016/j.chemosphere.2019.124642

17. Franklin A.M., Williams C.F., Watson J.E. Assessment of Soil to Mitigate Antibiotics in the Environment Due to Release of Wastewater Treatment Plant Effluent. J. Environ. Qual. 2018; 47 (6): 1347-1355. https://doi.org/10.2134/jeq2018.02.0076

18. Tran N.H., Hoang L., Nghiem L.D., Nguyen N.M.H., Ngo H.H., Guo W., Trinh Q.T., Mai N.H., Chen H., Nguyen D.D., Ta T.T., Gin K.Y. Occurrence and risk assessment of multiple classes of antibiotics in urban canals and lakes in Hanoi, Vietnam. Sci. Total. Environ. 2019; 692: 157-174. https://doi.org/10.1016/j.scitotenv.2019.07.092

19. Peixoto P.S., Toth I.V., Segundo M.A., Lima J.L.F.C. Fluoroquinolones and sulfonamides: Features of their determination in water. Review. Int. J. Environ. Anal. Chem. 2016; 96: 185-202.

20. Dmitrienko S.G., Kochuk E.V., Apyari V.V., Tolmacheva V.V., Zolotov Y.A. Recent advances in sam ple preparation techniques and methods of sulfonamides detection. A review. Anal. Chim. Acta. 2014; 850: 6-25. https://doi.org/10.1016/j.aca.2014.08.023

21. Xie X., Huang S., Zheng J., Ouyang G. Trends in sensitive detection and rapid removal of sulfonamides: A review. J. Sep. Sci. 2020; 43 (9-10): 1634-1652. https://doi.org/10.1002/jssc.201901341

22. Lahcen A.A., Amine A. Mini-Review: Recent Advances in Electrochemical Determination of Sulfonamides. Anal. Lett. 2018; 51: 424-441.

23. Guidance for Industry: Bioanalytical method validation. U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evolution and Research (CDER). Washington, DC; 2018: 41.

24. Guideline on validation of bioanalytical methods (draft). European Medicines Agency. Committee for medicinal products for human use. London; 2009: 23.