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Communication

Detection of Pharmaceutical Contamination in Amphipods of Lake Baikal by the HPLC-MS Method

by
Tamara Y. Telnova
†,
Maria M. Morgunova
†,
Sophie S. Shashkina
,
Anfisa A. Vlasova
,
Maria E. Dmitrieva
,
Victoria N. Shelkovnikova
,
Ekaterina V. Malygina
,
Natalia A. Imidoeva
,
Alexander Y. Belyshenko
,
Alexander S. Konovalov
,
Evgenia A. Misharina
and
Denis V. Axenov-Gribanov
*
Research Department, Biological and Soil Faculty, Irkutsk State University, Irkutsk 664003, Russia
*
Author to whom correspondence should be addressed.
†
These authors contributed equally to this work.
Antibiotics 2024, 13(8), 738; https://doi.org/10.3390/antibiotics13080738
Submission received: 29 June 2024 / Revised: 28 July 2024 / Accepted: 31 July 2024 / Published: 6 August 2024
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Versions Notes

Abstract

:
Pollution by active ingredients is one of the most significant and widespread forms of pollution on Earth. Medicines can have a negative impact on ecosystems, and contamination can have unpredictable consequences. An urgent and unexplored task is to study the Lake Baikal ecosystem and its organisms for the presence of trace concentrations of active pharmaceutical ingredients. Our study aimed to conduct a qualitative analysis of active pharmaceutical ingredients, and quantitative analysis of ibuprofen in endemic amphipods of Lake Baikal, using methods of high-performance liquid chromatography and mass spectrometry (HPLC-MS). Acetylsalicylic acid (aspirin), ibuprofen, acetaminophen, azithromycin, dimetridazole, metronidazole, amikacin, spiramycin, and some tetracycline antibiotics were detected in the studied littoral amphipods. We also detected different annual loads of active pharmaceutical ingredients on amphipods. Using the multiple reaction monitoring (MRM) mode mentioned in GOST International Technical Standards, we detected molecules, fragmented as amikacin, chlortetracycline, doxycycline, oxytetracycline, dimetridazole, metronidazole and spiramycin. Thus, we first revealed that invertebrates of Lake Baikal can uptake pharmaceutical contaminants in the environment.

Graphical Abstract

1. Introduction

Pollution of water bodies by various toxicants, pesticides, or drugs is one of the most significant environmental problems [1]. It is known that drugs can have negative effects on ecosystems, and pollution can cause unpredictable consequences in both the short and long term [2].
Pollution from active ingredients is closely linked to the increasing consumption of drugs by people [3]. This is fueled by such factors as demographic aging, high prevalence of chronic diseases, and the availability and emergence of new drugs. The nonregulated consumption of drugs by mankind leads to the penetration of drugs into domestic wastewater in unchanged form or as active metabolites [4].
Antimicrobial, antitumor, and antiviral drugs are top sellers in the global pharmaceutical market. Antibiotics are recognized as a group of drugs acting as environmental pollutants [5]. Previous studies have shown the presence of antibiotics in rivers [6,7], lakes [8,9], groundwater [10], invertebrates [11], and other environments. The mass and uncontrolled use of antibiotics contributes to a decrease in their effectiveness and the development of antibiotic resistance [12,13], increasing the burden on natural ecosystems.
Several studies have shown that drugs such as neomycin, trimethoprim, sulfamethoxazole and enrofloxacin have a high degree of toxicity against test cultures of Vibrio fischeri, Daphnia magna, Moina macrocopa and Oryzias latipes. Sulfamethazine, oxytetracycline, chlortetracycline, sulfadimethoxine and sulfathiazole are moderately toxic to organisms. Ampicillin and amoxicillin are the least toxic to the above organisms [14].
Drugs related to the non-steroidal anti-inflammatory class are also known to be toxic to inhabitants of aquatic ecosystems [15,16]. Diclofenac, ibuprofen, acetylsalicylic acid, naproxen, and acetaminophen have been reported to be present in different water bodies [17,18] as pharmaceutical pollutants. For example, acetaminophen has been detected in wastewater in Europe [19], USA [20], and the River Tyne (UK) [21]. Ibuprofen has been detected in the Llobregat River (Spain) [22], the Pearl River Delta (South China) [23] and in other locations by other publications.
Given this background information, effects of pharmaceutical pollution on ancient aquatic ecosystems may be dangerous, but are little studied. As hypothesized, active ingredients of drugs can reduce the biological diversity of endemic organisms that are highly sensitive to pharmaceutical agents [24]. Lake Baikal is an ancient water body and is a lake of tectonic origin in southeastern Siberia. The lake age is typically cited in the literature as 25–30 million years. However, extensive geological studies suggest that the geological age of Baikal is not less than 60 million years [25]. Baikal is the deepest lake on the planet and the largest natural reservoir of freshwater [26,27,28]. Currently, Lake Baikal is home to more than 2600 animal species and has a high rate of endemism [29]. The Baikal ecosystem is characterized by its structural and ecological complexity.
An urgent and unexplored task is to study the Lake Baikal ecosystem and its organisms for the presence of trace concentrations of active pharmaceutical ingredients. Notably, no monitoring observations regarding the detection of drugs in Baikal zoobenthos have been conducted to date. Invertebrate animals inhabiting the littoral zone of the lake are the first to encounter different pollutants and can accumulate them, thereby facilitating the migration of active ingredients along the food chains.
The aim of this study was to assess the contamination of Lake Baikal amphipods with active pharmaceutical ingredients using high-performance liquid chromatography and mass spectrometry.

2. Results

During the first stage of the study, we estimated the retention times of standard analyte solutions and achieved simultaneous detection of five analyzed components by selecting chromatographic conditions. The peak retention time for aspirin was 4.6 min, for azithromycin—2.9 min, for ibuprofen—5.7 min, for acetaminophen—0.5 min and for tetracycline—2.6 min. The variance of retention time was 0.05–0.07 min. Table 1 shows data on the presence of trace concentrations of active pharmaceutical ingredients in individual amphipods of Eulimnogammarus verrucosus species collected near Bolshoe Goloustnoe settlement in August 2020. Aspirin was detected in 10 out of 16 analyzed samples (level of contamination 63%; mean 0.62; SD 0.12; variance 0.25). Azithromycin and ibuprofen were found in 9 and 12 samples, respectively.
Then, we performed additional screening of drugs whose content in food products is regulated by GOST. The results of these analyses are presented in Table 2. The following precursor and product ions of drugs were detected in all 16 samples of amphipod species E. verrucosus: chlortetracycline, doxycycline, oxytetracycline and metronidazole. Selective molecular ions of amikacin, dimetridazole and spiramycin were detected in several samples of amphipods. Molecular ions of dimetridazole were detected in 11 out of 16 samples (level of contamination: 69%; mean 0.69; SD 0.12; variance 0.23). Molecular ions of spiramycin were detected in 4 samples (level of contamination: 25%; mean 0.25; SD 0.1; variance 0.20). Ions of amikacin were detected in 15 out of 16 samples (level of contamination: 94%; mean 0.93; SD 0.06; variance 0.06). Figure 1 shows the chromatograms of metronidazole, including the chromatograms of precursor and product ions. The typical raw data chromatograms of these analyses are presented in Supplementary Materials S1, Figures S1–S9.
At the same time, samples of E. verrucosus did not reveal selective molecular ions of the following substances: erythromycin, clarithromycin, tylosin, lincomycin, ampicillin, amoxicillin, florfenicol, thiamphenicol, sulfamethazine, sulfapyridine, gentamicin, hygromycin B, apramycin, and demeclocycline (Supplementary Materials S1, Figure S10).
The monitoring conducted at the same sampling point in 2020 and 2022 revealed differences in the pharmaceutical contamination of amphipod species. Based on the analysis of ibuprofen (Figure 2), we detected that almost 70% of E. verrucosus were contaminated in 2020, and 27% of E. verrucosus specimens were contaminated in 2022 (Tukey’s test p < 0.002; t-test p < 0.003; Kruskal–Wallis p < 0.003). Analysis of other pharmaceutical pollutants using MRM or selective mode was not performed in 2022.
The analysis revealed a significant relationship between the concentration of ibuprofen and the wet weight of E. verrucosus amphipods. The concentration of ibuprofen was found to be higher (p < 0.0001–p < 0.0004, two-way ANOVA) in small (juvenile, 0.1–0.2 g) amphipods than in the big (adult, 0.5–0.8 g) animals (Figure 3). Thus, E. verrucosus amphipods with up to 0.2 g wet weight contained ibuprofen in concentrations ranging from 74.71 to 166.38 ng/g. Amphipods with a wet weight of 0.2 to 0.5 g contained ibuprofen in concentrations ranging from 18.50 to 61.75 ng/g. Finally, amphipods with a wet weight above 0.7 g were characterized by ibuprofen concentrations in the range of 14.92–16.98 ng/g.

3. Discussion

This study confirmed the hypothesis regarding contamination of Lake Baikal zoobenthos representatives, using amphipods as an example, with active pharmaceutical ingredients, or their selective molecular ions. Contamination of the Lake Baikal ecosystem and its amphipods by active pharmaceutical ingredients is a significant and urgent problem. However, only a small number of studies have been published to date that characterize pollution of Lake Baikal by active pharmaceutical ingredients.
Studies conducted by Meyer M. F. et al. (2021, 2022) found the presence of pharmaceutical agents such as acetaminophen, paraxanthine, caffeine, cotinine, cimetidine, diphenhydramine, phenazone, and sulfachloropyridazine in Lake Baikal water. Other ingredients, such as amphetamine, morphine, carbamazepine, tenamphetamine, methamphetamine, thiabendazole, methylenedioxymethamphetamine, sulfamethazine, sulfamethoxazole, and trimethoprim were not detected [30,31].
Our study shows that each of 16 samples of E. verrucosus collected in B. Goloustnoe settlement in August 2020 contains at least five drug contaminants. Additionally, ibuprofen was detected in samples collected in 2022 (N = 44). Thus, the presence of aspirin, acetaminophen, tetracycline, azithromycin and ibuprofen in amphipods was confirmed. However, different levels of contamination and the absence of quantitative data do not allow us to assume pathways for the transformation and migration of active pharmaceutical ingredients through the ecosystem.
The presence of active pharmaceutical ingredients in the endemic amphipods of E. verrucosus species can be explained by their entry into the ecosystem through sewage or groundwater [32]. For example, paracetamol (acetaminophen), ibuprofen and azithromycin are of synthetic origin, and are widely used in medicine, veterinary medicine and households [33,34,35,36].
Detection of these molecular ions of drugs in amphipods may indicate their regular entry into domestic wastewater in unchanged form. For instance, acetaminophen has been previously detected in water [30], suggesting that this active ingredient is regularly released into the ecosystem of Lake Baikal. The presence of other pharmaceutical contaminants, such as dimetridazole, metronidazole, and amikacin, may be attributed to the successful use of antibiotics in livestock to treat and prevent infectious diseases [37,38,39,40].
In addition to their synthetic origin, active ingredients of drugs can also be obtained naturally. For example, acetylsalicylic acid is a derivative of salicylic acid, which is the active ingredient in willow [38], raspberry, blackberry and blackcurrant extracts [41]. Thus, aspirin can enter the water not only with sewage but also with particles of bark and leaves of plants containing salicylate. Thus, amphipods, being phyto- and detritophagous [42], could consume these natural products with food, as Baikal algae, whose chemistry of natural products is not studied.
Additionally, some naturally occurring active ingredients can be detected due to symbiotic microorganisms living in the gastrointestinal tract or hemolymph of amphipods. These microorganisms are capable of producing natural compounds. For example, tetracycline is a semi-synthetic antibiotic and can also be produced by actinobacteria related to Streptomyces aureofaciens and S. rimosus. These microorganisms are regular symbionts of amphipods [43,44,45]. Notably, oxytetracycline, doxycycline and chlortetracycline, identified during the study, also belong to the tetracycline group. Spiramycin refers to natural antibiotics in the macrolide group and is synthesized by actinobacteria of species Streptomyces ambofaciens [46,47].
Thus, our study demonstrates that the amphipods of Lake Baikal can uptake pharmaceutical contaminants in their environment. Although the stress response of Baikal-endemic amphipods to heavy metals [48,49], natural organic matter [50], or model organic pollutant [51] is well studied, the relationship of Baikal amphipods to pharmaceutical contaminants has never been investigated. Additionally, pharmaceutical pollutants can have toxic effects on aquatic organisms [52,53,54] and induce oxidative stress [55,56]. Pharmaceutical pollutants can also lead to a decrease in biodiversity, which is especially relevant for the ancient Lake Baikal [57]. The problem acquires particular urgency and significance in view of the tolerance of blue-green algae to ibuprofen, a typical pharmaceutical pollutant, and the effects of blue-green algae growth regularly observed in Lake Baikal [32]. Thus, assessing pharmaceutical contamination of ancient ecosystems and studying the response of endemic organisms can help answer global questions, including those related to climate change, antibiotic resistance, and the overall human impact on the planet.

4. Materials and Methods

Amphipods (Amphipoda, Crustacea) were chosen as the subject of our study. Amphipods are one of the most diverse groups of organisms in Lake Baikal, with taxonomic diversity and different ecological preferences. To date, the endemic fauna of Baikal amphipods is represented by more than 350 endemic species and subspecies [42].
For this study, we selected amphipods of the species Eulimnogammarus verrucosus (Gerstf., 1858). Samples were collected with a hydrobiological net on the stone littoral at a depth of 0.1–0.5 m near Bolshoe Goloustnoe settlement in August 2020 and 2022. Bolshoe Goloustnoe is a settlement located 120 km from Irkutsk, and it is a representative Baikal settlement with moderate anthropogenic, agricultural and touristic load. Each amphipod was fixed at the sampling site into disposable and sterile Eppendorf microtubes. Each amphipod was placed in a separate tube and frozen at −20 °C.
In the laboratory, each individual was weighed using an analytical scale (Sartogosm CE224-C, St. Petersburg, Russia). The wet weight of the amphipods was 0.1–0.7 g and their average weight was 0.28 g. The samples were further homogenized using vibration ball mill in the presence of acetonitrile at the ratio of 1:10 (1—weight of amphipods, g; 10—volume of acetonitrile, mL). Each sample contained one individual crustacean. The obtained homogenate was centrifuged for 10 min at 3000× g rpm (Armed LC04B, St. Petersburg, Russia). Then 800 μL of supernatant was transferred to microtubes and protein precipitation was performed by adding 10% trichloroacetic acid solution in a volume of 80 μL. Then, microtubes were centrifuged again for 10 min at 16,000× g rpm (Biosan Microspin-12, Riga, Latvia). The prepared samples were stored at +4 °C. Prior to analysis, the samples were filtered through a 13 mm diameter, 45 µm pore size syringe filter with PVDF membrane, and then 100 µL of the filtrate was transferred into chromatographic vials. The extracts were diluted with 900 µL of acetonitrile [58,59,60].
In this study, we prepared standardized samples of active pharmaceutical ingredients on our own by extracting them from drugs. For qualitative analysis, solutions of aspirin, acetaminophen, ibuprofen, tetracycline, and azithromycin were made from crushed tablets. Analytical standards of ibuprofen (11559-2020, NCAS, Moscow, Russia) and azithromycin (11570-2020, NCAS, Moscow, Russia) were used as additional reference positive control. The reference positive control of ibuprofen was used in concentration of 72 ng/mL and added to extracts of amphipods. Methyl alcohol served as the solvent. The solutions prepared from analytical standards and from crushed tablets were used to determine correct ionization and fragmentation parameters for molecules of the analyzed active ingredients [61,62]. Additionally, these solutions were used to assess the suitability of chromatographic systems and to establish retention times. To avoid false-positive results, we used the method involving the analysis of natural sample, analytical control and the analysis of a sample with a standard control added to it. The negative control was a mixture of solvents and rinses that are used to rinse Eppendorf tubes and filters [62,63,64].
A qualitative analysis of the content of other active ingredients was conducted using the multiple reaction monitoring (MRM) mode [65,66,67]. The MRM transitions of the studied drugs were described using GOST standards (Gosudarstvennyy Standart, a set of international technical standards maintained by the Euro-Asian Council for Standardization, Metrology and Certification for the Commonwealth of Independent States), which are employed for the control of active ingredients in composition of food products and food raw materials (Table 3).
Screening for the presence of active ingredients in samples of Baikal-endemic amphipods was performed using the Agilent Infinity II (2019) chromatography mass spectrometry system with an Agilent 6470B triple quadrupole mass spectrometry detector (Supplementary Materials S1, Figure S11). Agilent Poroshell C18 chromatographic column 2.1 × 50 mm; column temperature −30 °C. Table 4 presents the program for HPLC separation used for the general screening (qualitative data). Table 5 presents the program for HPLC separation of samples containing ibuprofen (quantitative data). Mass spectrometer setup program: ion source gas temperature: 300 °C; ion source gas flow: 5 L/min; nebuliser: 45 psi; drying gas temperature: 250 °C; drying gas flow: 11 L/min; capillary voltage: 3500 V; sample volume: 1 µL.
During the study, over 60 samples of individually collected amphipods were analyzed. In total, over the period 2020–2024, more than 200 samples of amphipods were collected and analyzed. Here, we present the first structured data related to the first qualitative data characterizing pharmaceutical contamination detected in amphipods species of E. verrucosus, collected in the settlement of BS. Goloustnoe in August 2020 (N = 16) and 2022 (N = 44). Each analyzed sample contained one individual crustacean. The analysis of each sample was conducted three times.
The statistical processing was performed in Past software (V4.03) using the Kruskal–Wallis H test (one-way ANOVA on ranks as a non-parametric method) for the analysis of qualitative data. The Bonferroni sequential significance model was used. One-way ANOVA, t-test and F-test were used to analyze quantitative data. The effects of factors “year of sampling” and “wet weight of amphipods” were reported based on two-way ANOVA. To determine which group means were significantly different from each other, Tukey’s post-hoc tests were performed (Supplementary Materials S2). Differences between the mean values of the parameters were considered significant at p ≤ 0.05.

5. Conclusions

Our study reveals that endemic amphipods (E. verrucosus) in Lake Baikal are contaminated with active pharmaceutical ingredients and this is the first report showing that invertebrates in Lake Baikal contain such contaminants. The presence of ibuprofen, acetaminophen, tetracycline and other pharmaceuticals may have a negative impact on the endemic organisms of Lake Baikal. For this reason, monitoring the concentrations of these pharmaceuticals and investigating their effects on Lake Baikal organisms are necessary.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/antibiotics13080738/s1.

Author Contributions

Conceptualization: D.V.A.-G., T.Y.T. and E.A.M.; methodology: M.M.M. and A.S.K.; validation: M.M.M., A.S.K., S.S.S. and E.A.M.; formal analysis and investigation: T.Y.T., M.M.M., S.S.S., A.A.V., M.E.D., V.N.S., E.V.M., N.A.I. and A.Y.B.; resources: D.V.A.-G. and E.A.M.; writing (original draft preparation) T.Y.T. and M.M.M.; writing (review and editing) E.A.M., D.V.A.-G. and A.S.K.; visualization, A.Y.B.; supervision: D.V.A.-G. and M.M.M.; project administration: D.V.A.-G.; funding acquisition: E.A.M. and D.V.A.-G. All authors have read and agreed to the published version of the manuscript.

Funding

The study was carried out with the financial support of the project of the Ministry of Higher Education and Science of the Russian Federation (projects FZZE 2024-0003, FZZE 2024-0011).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The original contributions presented in the study are included in the article (and Supplementary Material), further inquiries can be directed to the corresponding authors.

Acknowledgments

The authors gratefully thank reviewers of this article for their constructive comments and suggestions.

Conflicts of Interest

The authors declare no conflicts of interest.

References

  1. Rathi, B.S.; Kumar, P.S.; Vo, D.V.N. Critical Review on Hazardous Pollutants in Water Environment: Occurrence, Monitoring, Fate, Removal Technologies and Risk Assessment. Sci. Total Environ. 2021, 797, 149134. [Google Scholar] [CrossRef] [PubMed]
  2. Khan, S.; Naushad, M.; Govarthanan, M.; Iqbal, J.; Alfadul, S.M. Emerging Contaminants of High Concern for the Environment: Current Trends and Future Research. Environ. Res. 2022, 207, 112609. [Google Scholar] [CrossRef] [PubMed]
  3. Vaudin, P.; Augé, C.; Just, N.; Mhaouty-Kodja, S.; Mortaud, S.; Pillon, D. When Pharmaceutical Drugs Become Environmental Pollutants: Potential Neural Effects and Underlying Mechanisms. Environ. Res. 2022, 205, 112495. [Google Scholar] [CrossRef] [PubMed]
  4. Grela, A.; Kuc, J.; Bajda, T. A Review on the Application of Zeolites and Mesoporous Silica Materials in the Removal of Non-Steroidal Anti-Inflammatory Drugs and Antibiotics from Water. Materials 2021, 14, 4994. [Google Scholar] [CrossRef] [PubMed]
  5. Bilal, M.; Mehmood, S.; Rasheed, T.; Iqbal, H.M.N. Antibiotics Traces in the Aquatic Environment: Persistence and Adverse Environmental Impact. Curr. Opin. Environ. Sustain. 2020, 13, 68–74. [Google Scholar] [CrossRef]
  6. Johnson, A.C.; Keller, V.; Dumont, E.; Sumpter, J.P. Assessing the Concentrations and Risks of Toxicity from the Antibiotics Ciprofloxacin, Sulfamethoxazole, Trimethoprim and Erythromycin in European Rivers. Sci. Total Environ. 2015, 511, 747–755. [Google Scholar] [CrossRef] [PubMed]
  7. Zhang, L.; Zhang, C.; Lian, K.; Ke, D.; Xie, T.; Liu, C. River Restoration Changes Distributions of Antibiotics, Antibiotic Resistance Genes, and Microbial Community. Sci. Total Environ. 2021, 788, 147873. [Google Scholar] [CrossRef] [PubMed]
  8. Yang, Y.; Song, W.; Lin, H.; Wang, W.; Du, L.; Xing, W. Antibiotics and Antibiotic Resistance Genes in Global Lakes: A Review and Meta-Analysis. Environ. Int. 2018, 116, 60–73. [Google Scholar] [CrossRef]
  9. 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.; et al. Occurrence and Risk Assessment of Multiple Classes of Antibiotics in Urban Canals and Lakes in Hanoi, Vietnam. Sci. Total Environ. 2019, 692, 157–174. [Google Scholar] [CrossRef]
  10. Wu, S.; Hua, P.; Gui, D.; Zhang, J.; Ying, G.; Krebs, P. Occurrences, Transport Drivers, and Risk Assessments of Antibiotics in Typical Oasis Surface and Groundwater. Water Res. 2022, 225, 119138. [Google Scholar] [CrossRef]
  11. Liu, L.; Wu, W.; Zhang, J.; Lv, P.; Xu, L.; Yan, Y. Progress of Research on the Toxicology of Antibiotic Pollution in Aquatic Organisms. Acta Ecol. Sin. 2018, 38, 36–41. [Google Scholar] [CrossRef]
  12. Martinez, J.L. Environmental Pollution by Antibiotics and by Antibiotic Resistance Determinants. Environ. Pollut. 2009, 157, 2893–2902. [Google Scholar] [CrossRef] [PubMed]
  13. Kotwani, A.; Joshi, J.; Kaloni, D. Pharmaceutical Effluent: A Critical Link in the Interconnected Ecosystem Promoting Antimicrobial Resistance. Environ. Sci. Pollut. Res. 2021, 28, 32111–32124. [Google Scholar] [CrossRef]
  14. Park, S.; Choi, K. Hazard Assessment of Commonly Used Agricultural Antibiotics on Aquatic Ecosystems. Ecotoxicology 2008, 17, 526–538. [Google Scholar] [CrossRef] [PubMed]
  15. Rastogi, A.; Tiwari, M.K.; Ghangrekar, M.M. A Review on Environmental Occurrence, Toxicity and Microbial Degradation of Non-Steroidal Anti-Inflammatory Drugs (Nsaids). J. Environ. Manag. 2021, 300, 113694. [Google Scholar] [CrossRef] [PubMed]
  16. da Silva, T.L.; Costa, C.S.D.; da Silva, M.G.C.; Vieira, M.G.A. Overview of Non-Steroidal Anti-Inflammatory Drugs Degradation by Advanced Oxidation Processes. J. Clean. Prod. 2022, 346, 131226. [Google Scholar] [CrossRef]
  17. Aydin, S.; Aydin, M.E.; Ulvi, A. Monitoring the Release of Anti-Inflammatory and Analgesic Pharmaceuticals in the Receiving Environment. Environ. Sci. Pollut. Res. 2019, 26, 36887–36902. [Google Scholar] [CrossRef] [PubMed]
  18. Castro-Pastrana, L.I.; Palacios-Rosas, E.; Toledo-Wall, M.L.; Cerro-López, M. Worldwide Occurrence, Detection, and Fate of Nonsteroidal Anti-Inflammatory Drugs in Water. In Non-Steroidal Anti-Inflammatory Drugs in Water: Emerging Contaminants and Ecological Impact; Gómez-Oliván, L.M., Ed.; Springer International Publishing: Geneva, Switzerland, 2020; pp. 55–82. ISBN 978-3-030-56294-6. [Google Scholar]
  19. Ternes, T.A. Occurrence of Drugs in German Sewage Treatment Plants and Rivers. Water Res. 1998, 32, 3245–3260. [Google Scholar] [CrossRef]
  20. Kolpin, D.W.; Furlong, E.T.; Meyer, M.T.; Thurman, E.M.; Zaugg, S.D.; Barber, L.B.; Buxton, H.T. Pharmaceuticals, Hormones, and Other Organic Wastewater Contaminants in U.S. Streams, 1999–2000: A National Reconnaissance. Environ. Sci. Technol. 2002, 36, 1202–1211. [Google Scholar] [CrossRef]
  21. Gómez-Oliván, L.M.; Galar-Martínez, M.; García-Medina, S.; Valdés-Alanís, A.; Islas-Flores, H.; Neri-Cruz, N. Genotoxic Response and Oxidative Stress Induced by Diclofenac, Ibuprofen and Naproxen in Daphnia magna. Drug Chem. Toxicol. 2014, 37, 391–399. [Google Scholar] [CrossRef]
  22. Ginebreda, A.; Muñoz, I.; de Alda, M.L.; Brix, R.; López-Doval, J.; Barceló, D. Environmental Risk Assessment of Pharmaceuticals in Rivers: Relationships between Hazard Indexes and Aquatic Macroinvertebrate Diversity Indexes in the Llobregat River (NE Spain). Environ. Int. 2010, 36, 153–162. [Google Scholar] [CrossRef] [PubMed]
  23. Zhao, J.L.; Ying, G.G.; Liu, Y.S.; Chen, F.; Yang, J.F.; Wang, L.; Yang, X.B.; Stauber, J.L.; Warne, M.S.J. Occurrence and a Screening-Level Risk Assessment of Human Pharmaceuticals in the Pearl River System, South China. Environ. Toxicol. Chem. 2010, 29, 1377–1384. [Google Scholar] [CrossRef] [PubMed]
  24. Néstor, M.C.; Mariana, C. Impact of Pharmaceutical Waste on Biodiversity. In Ecopharmacovigilance: Multidisciplinary Approaches to Environmental Safety of Medicines; Gómez-Oliván, L.M., Ed.; Springer International Publishing: Geneva, Switzerland, 2019; pp. 235–253. ISBN 978-3-319-73476-7. [Google Scholar]
  25. Matz, V.D.; Efimova, I.M. Geological History of Baikal. Nature 2017, 3, 13–27. (In Russian) [Google Scholar]
  26. Rusinek, O.T.; Takhteev, V.V.; Gladkochub, D.P.; Khodzher, T.V.; Budnev, N.M. Baikal Science; Nauka Publishers: Moscow, Russia, 2012; pp. 641–1019. (In Russian) [Google Scholar]
  27. Moore, M.V.; Hampton, S.E.; Izmest’eva, L.R.; Silow, E.A.; Peshkova, E.V.; Pavlov, B.K. Climate change and the world’s “sacred sea”—Lake Baikal, Siberia. BioScience 2009, 59, 405–417. [Google Scholar] [CrossRef]
  28. Moore, M.V.; De Stasio, B.T., Jr.; Huizenga, K.N.; Silow, E.A. Trophic coupling of the microbial and the classical food web in Lake Baikal, Siberia. Freshw. Biol. 2019, 64, 138–151. [Google Scholar] [CrossRef]
  29. Timoshkin, O.A.; Samsonov, D.P.; Yamamuro, M.; Moore, M.V.; Belykh, O.I.; Malnik, V.V.; Sakirko, M.V.; Shirokaya, A.A.; Bondarenko, N.A.; Domysheva, V.M.; et al. Rapid Ecological Change in the Coastal Zone of Lake Baikal (East Siberia): Is the Site of the World’s Greatest Freshwater Biodiversity in Danger? J. Great Lakes Res. 2016, 42, 487–497. [Google Scholar] [CrossRef]
  30. Meyer, M.F.; Ozersky, T.; Woo, K.H.; Shchapov, K.; Galloway, A.W.; Schram, J.B.; Snow, D.D.; Timofeyev, M.A.; Karnaukhov, D.Y.; Brousil, M.R.; et al. A unified dataset of co-located sewage pollution, periphyton, and benthic macroinvertebrate community and food web structure from Lake Baikal (Siberia). Limnol. Oceanogr. Lett. 2021, 7, 62–79. [Google Scholar] [CrossRef]
  31. Meyer, M.; Ozersky, T.; Woo, K.; Shchapov, K.; Galloway, A.; Schram, J.; Rosi, E.; Snow, D.; Timofeyev, M.; Karnaukhov, D.; et al. Effects of Spatially Heterogeneous Lakeside Development on Nearshore Biotic Communities in a Large, Deep, Oligotrophic Lake. Limnol. Oceanogr. 2022, 67, 2649–2664. [Google Scholar] [CrossRef]
  32. Timoshkin, O.A.; Moore, M.V.; Kulikova, N.N.; Tomberg, I.V.; Malnik, V.V.; Shimaraev, M.N.; Troitskaya, E.S.; Shirokaya, A.A.; Sinyukovich, V.N.; Zaitseva, E.P.; et al. Groundwater Contamination by Sewage Causes Benthic Algal Outbreaks in the Littoral Zone of Lake Baikal (East Siberia). J. Great Lakes Res. 2018, 44, 230–244. [Google Scholar] [CrossRef]
  33. Freo, U.; Ruocco, C.; Valerio, A.; Scagnol, I.; Nisoli, E. Paracetamol: A Review of Guideline Recommendations. J. Clin. Med. 2021, 10, 3420. [Google Scholar] [CrossRef]
  34. Oliver, M.E.; Hinks, T.S.C. Azithromycin in Viral Infections. Rev. Med. Virol. 2021, 31, e2163. [Google Scholar] [CrossRef] [PubMed]
  35. Bello, A.M.; Dye, C. Current Perceptions and Use of Paracetamol in Dogs among Veterinary Surgeons Working in the United Kingdom. J. Vet. Med. Sci. 2023, 9, 679–686. [Google Scholar] [CrossRef] [PubMed]
  36. Chalifoux, N.V.; Butty, E.M.; Mauro, K.D.; Moyle, R.B.; Ehrhardt, C.M.; Robertson, J.B.; Labato, M.A.; Culler, C.A.; Londoño, L.A.; Vigani, A.; et al. Outcomes of 434 Dogs with Non-Steroidal Anti-Inflammatory Drug Toxicosis Treated with Fluid Therapy, Lipid Emulsion, or Therapeutic Plasma Exchange. J. Vet. Intern. Med. 2023, 37, 161–172. [Google Scholar] [CrossRef] [PubMed]
  37. Stephens, L.R.; Slee, K.J. Metronidazole for the Treatment of Bovine Pyometra. Aust. Vet. J. 1987, 64, 343–346. [Google Scholar] [CrossRef] [PubMed]
  38. Granja, R.H.M.M.; Nino, A.M.M.; Reche, K.V.G.; Giannotti, F.M.; de Lima, A.C.; Wanschel, A.C.B.A.; Salerno, A.G. Determination and Confirmation of Metronidazole, Dimetridazole, Ronidazole and Their Metabolites in Bovine Muscle by LC-MS/MS. Food Addit. Contam. Part. A 2013, 30, 970–976. [Google Scholar] [CrossRef] [PubMed]
  39. Motos, A.; Yang, H.; Li Bassi, G.; Yang, M.; Meli, A.; Battaglini, D.; Cabrera, R.; Bobi, J.; Pagliara, F.; Frigola, G.; et al. Inhaled Amikacin for Pneumonia Treatment and Dissemination Prevention: An Experimental Model of Severe Monolateral Pseudomonas Aeruginosa Pneumonia. Crit. Care 2023, 27, 60. [Google Scholar] [CrossRef] [PubMed]
  40. Adamczak, A.; Ożarowski, M.; Karpiński, T.M. Antibacterial Activity of Some Flavonoids and Organic Acids Widely Distributed in Plants. J. Clin. Med. 2020, 9, 109. [Google Scholar] [CrossRef] [PubMed]
  41. Jeffreys, D. Aspirin: The Remarkable Story of a Wonder Drug; Bloomsbury: New York, NY, USA, 2004; ISBN 978-1-58234-386-0. [Google Scholar]
  42. Takhteev, V. On the current state of taxonomy of the Baikal Lake amphipods (Crustacea: Amphipoda) and the typological ways of constructing their system. Arthropoda Sel. 2019, 28, 374–402. [Google Scholar] [CrossRef]
  43. Axenov-Gribanov, D.; Rebets, Y.; Tokovenko, B.; Voytsekhovskaya, I.; Timofeyev, M.; Luzhetskyy, A. The Isolation and Characterization of Actinobacteria from Dominant Benthic Macroinvertebrates Endemic to Lake Baikal. Folia Microbiol. 2016, 61, 159–168. [Google Scholar] [CrossRef]
  44. Protasov, E.S.; Axenov-Gribanov, D.V.; Rebets, Y.V.; Voytsekhovskaya, I.V.; Tokovenko, B.T.; Shatilina, Z.M.; Luzhetskyy, A.; Timofeyev, M.A. The diversity and antibiotic properties of actinobacteria associated with endemic deepwater amphipods of Lake Baikal. Anton Leeuw. Int. J. 2017, 110, 1593–1611. [Google Scholar] [CrossRef]
  45. Olano, C.; Rodríguez, M. Actinomycetes Associated with Arthropods as a Source of New Bioactive Compounds. CIMB 2024, 46, 3822–3838. [Google Scholar] [CrossRef] [PubMed]
  46. Quinn, G.A.; Banat, A.M.; Abdelhameed, A.M.; Banat, I.M. Streptomyces from traditional medicine: Sources of new innovations in antibiotic discovery. J. Med. Microbiol. 2020, 69, 1040–1048. [Google Scholar] [CrossRef]
  47. Risdian, C.; Mozef, T.; Wink, J. Biosynthesis of Polyketides in Streptomyces. Microorganisms 2019, 7, 124. [Google Scholar] [CrossRef]
  48. Jakob, L.; Bedulina, D.S.; Axenov-Gribanov, D.V.; Ginzburg, M.; Shatilina, Z.M.; Lubyaga, Y.A.; Madyarova, E.V.; Gurkov, A.N.; Timofeyev, M.A.; Pörtner, H.-O.; et al. Uptake Kinetics and Subcellular Compartmentalization Explain Lethal but Not Sublethal Effects of Cadmium in Two Closely Related Amphipod Species. Available online: https://pubs.acs.org/doi/abs/10.1021/acs.est.6b06613 (accessed on 19 July 2024).
  49. Pavlichenko, V.V.; Protopopova, M.V.; Timofeyev, M.; Luckenbach, T. Identification of a Putatively Multixenobiotic Resistance Related Abcb1 Transporter in Amphipod Species Endemic to the Highly Pristine Lake Baikal. Environ. Sci. Pollut. Res. 2015, 22, 5453–5468. [Google Scholar] [CrossRef] [PubMed]
  50. Timofeyev, M.A.; Steinberg, C.E.W. Antioxidant Response to Natural Organic Matter (NOM) Exposure in Three Baikalean Amphipod Species from Contrasting Habitats. Comp. Biochem. Physiol. B Biochem. Mol. Biol. 2006, 145, 197–203. [Google Scholar] [CrossRef] [PubMed]
  51. Shatilina, Z.; Drozdova, P.; Bedulina, D.; Rivarola-Duarte, L.; Schreiber, S.; Otto, C.; Jühling, F.; Aulhorn, S.; Busch, W.; Lubyaga, Y.; et al. Transcriptome-Level Effects of the Model Organic Pollutant Phenanthrene and Its Solvent Acetone in Three Amphipod Species. Comp. Biochem. Physiol. Part D Genom. Proteom. 2020, 33, 100630. [Google Scholar] [CrossRef]
  52. Mohd Zanuri, N.B.; Bentley, M.G.; Caldwell, G.S. Assessing the Impact of Diclofenac, Ibuprofen and Sildenafil Citrate (Viagra®) on the Fertilisation Biology of Broadcast Spawning Marine Invertebrates. Mar. Environ. Res. 2017, 127, 126–136. [Google Scholar] [CrossRef] [PubMed]
  53. Grzesiuk, M.; Wacker, A.; Spijkerman, E. Photosynthetic Sensitivity of Phytoplankton to Commonly Used Pharmaceuticals and Its Dependence on Cellular Phosphorus Status. Ecotoxicology 2016, 25, 697–707. [Google Scholar] [CrossRef]
  54. Du, J.; Mei, C.; Ying, G.; Xu, M. Toxicity Thresholds for Diclofenac, Acetaminophen and Ibuprofen in the Water Flea Daphnia Magna. Bull. Environ. Contam. Toxicol. 2016, 97, 84–90. [Google Scholar] [CrossRef]
  55. Sun, C.; Dudley, S.; Trumble, J.; Gan, J. Pharmaceutical and Personal Care Products-Induced Stress Symptoms and Detoxification Mechanisms in Cucumber Plants. Environ. Pollut. 2018, 234, 39–47. [Google Scholar] [CrossRef]
  56. Bouzidi, I.; Fkiri, A.; Saidani, W.; Khazri, A.; Mezni, A.; Mougin, K.; Beyrem, H.; Sellami, B. The Pharmaceutical Triclosan Induced Oxidative Stress and Physiological Disorder in Marine Organism and Nanoparticles as a Potential Mitigating Tool. Mar. Environ. Res. 2024, 196, 106424. [Google Scholar] [CrossRef] [PubMed]
  57. Farkas, R.; Mireisz, T.; Toumi, M.; Abbaszade, G.; Sztráda, N.; Tóth, E. The Impact of Anti-Inflammatory Drugs on the Prokaryotic Community Composition and Selected Bacterial Strains Based on Microcosm Experiments. Microorganisms 2023, 11, 1447. [Google Scholar] [CrossRef]
  58. Bashyal, S. Ibuprofen and its different analytical and manufacturing methods: A review. Asian J. Pharm. Clin. Res. 2018, 11, 25–29. [Google Scholar] [CrossRef]
  59. Bragança, I.; Plácido, A.; Paíga, P.; Domingues, V.F.; Delerue-Matos, C. QuEChERS: A New Sample Preparation Approach for the Determination of Ibuprofen and Its Metabolites in Soils. Sci. Total Environ. 2012, 433, 281–289. [Google Scholar] [CrossRef]
  60. Dowling, G.; Gallo, P.; Fabbrocino, S.; Serpe, L.; Regan, L. Determination of Ibuprofen, Ketoprofen, Diclofenac and Phenylbutazone in Bovine Milk by Gas Chromatography-Tandem Mass Spectrometry. Food Addit. Contam. Part A 2008, 25, 1497–1508. [Google Scholar] [CrossRef] [PubMed]
  61. USP-NF. Available online: https://www.uspnf.com/sites/default/files/usp_pdf/EN/USPNF/errata467Ibuprofen.pdf (accessed on 28 June 2024).
  62. Eraga, S.O.; Arhewoh, M.I.; Chibuogwu, R.N.; Iwuagwu, M.A. A Comparative UV−HPLC Analysis of Ten Brands of Ibuprofen Tablets. Asian Pac. J. Trop. Biomed. 2015, 5, 880–884. [Google Scholar] [CrossRef]
  63. ICH Harmonised Tripartite Guideline. Q2(R1) Validation of Analytical Procedures: Text and Methodology; ICH: London, UK, 2005; pp. 1–13. [Google Scholar]
  64. Riley, C.M.; Rosanske, T.W.; Reid, G.L. Specification of Drug Substances and Products: Development and Validation of Analytical Methods, 2nd ed.; Elsevier: New York, NY, USA, 2020; pp. 10–495. ISBN 9780081028247. [Google Scholar]
  65. Wang, C.; Wang, Y.; Xie, H.; Zhan, C.; He, X.; Liu, R.; Hu, R.; Shen, J.; Jia, Y. Establishment and Validation of an SIL-IS LC–MS/MS Method for the Determination of Ibuprofen in Human Plasma and Its Pharmacokinetic Study. Biomed. Chromatogr. 2022, 36, e5287. [Google Scholar] [CrossRef]
  66. Borges, K.B.; de Oliveira, A.R.M.; Barth, T.; Jabor, V.A.P.; Pupo, M.T.; Bonato, P.S. LC–MS–MS Determination of Ibuprofen, 2-Hydroxyibuprofen Enantiomers, and Carboxyibuprofen Stereoisomers for Application in Biotransformation Studies Employing Endophytic Fungi. Anal. Bioanal. Chem. 2011, 399, 915–925. [Google Scholar] [CrossRef]
  67. Puangpetch, A.; Limrungsikul, A.; Prommas, S.; Rukthong, P.; Sukasem, C. Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method for Determination of Ibuprofen in Human Plasma. Clin. Mass Spectrom. 2020, 15, 6–12. [Google Scholar] [CrossRef]
  68. Martignac, M.; Oliveros, E.; Maurette, M.-T.; Claparols, C.; Benoit-Marquié, F. Mechanistic Pathways of the Photolysis of Paracetamol in Aqueous Solution: An Example of Photo-Fries Rearrangement. Photochem. Photobiol. Sci. 2013, 12, 527–535. [Google Scholar] [CrossRef]
  69. GOST 32798-2014; Food Products, Food Raw Materials. Method for Determination of the Aminoglycosides Content by High Performance Liquid Chromatography with Mass Spectrometry Detector. Rosstandart: Moscow, Russia, 2016. (In Russian)
  70. GOST 34533-2019; Food Products, Food Raw Materials. Method for Determination of Sulfonamides, Nitroimidazoles, Penicillins, Amphenicols by High Performance Liquid Chromatography-Mass Spectrometry. Rosstandart: Moscow, Russia, 2020. (In Russian)
  71. Polagani, S.R.; Pilli, N.R.; Gandu, V. High Performance Liquid Chromatography Mass Spectrometric Method for the Simultaneous Quantification of Pravastatin and Aspirin in Human Plasma: Pharmacokinetic Application. J. Pharm. Anal. 2012, 2, 206–213. [Google Scholar] [CrossRef] [PubMed]
  72. Chen, L.; Qin, F.; Ma, Y.; Li, F. Quantitative Determination of Azithromycin in Human Plasma by Ultra Performance Liquid Chromatography–Electrospray Ionization Mass Spectrometry and Its Application in a Pharmacokinetic Study. J. Chromatogr. B. 2007, 855, 255–261. [Google Scholar] [CrossRef] [PubMed]
  73. GOST 31694-2012; Food Products, Food Raw Materials. Method of Determination of the Antibiotic Residues of Tetracycline Group by High Performance Liquid Chromatography—Mass Spectrometry. Rosstandart: Moscow, Russia, 2013. (In Russian)
  74. GOST 34136-2017; Food Products, Food Raw Materials. Method for Determination of the Residual Content of Macrolides, Lincosamides and Pleuromutilins by High Performance Liquid Chromatography—Mass spectrometry. Rosstandart: Moscow, Russia, 2018. (In Russian)
  75. GOST 32881-2014; Food Products, Food Raw Materials. Method for Determination of the Non-Steroidal Anti-Inflammatory Drug Residue Content by High Performance Liquid Chromatography—Mass Spectrometry. Rosstandart: Moscow, Russia, 2016. (In Russian)
Antibiotics 13 00738 g001
Figure 1. Chromatogram of metronidazole detected in samples of amphipod E. verrucosus (2020).
Figure 1. Chromatogram of metronidazole detected in samples of amphipod E. verrucosus (2020).
Antibiotics 13 00738 g001
Antibiotics 13 00738 g002
Figure 2. Chromatogram of ibuprofen detected in samples of amphipod E. verrucosus.
Figure 2. Chromatogram of ibuprofen detected in samples of amphipod E. verrucosus.
Antibiotics 13 00738 g002
Antibiotics 13 00738 g003
Figure 3. Correlation between concentration of ibuprofen and the wet weight of species E. verrucosus amphipods, ng/g (white marker—2020; black marker—2022).
Figure 3. Correlation between concentration of ibuprofen and the wet weight of species E. verrucosus amphipods, ng/g (white marker—2020; black marker—2022).
Antibiotics 13 00738 g003
Table 1. The presence of active of pharmaceutical ingredients in samples of individual amphipods of E. verrucosus species collected in August 2020.
Table 1. The presence of active of pharmaceutical ingredients in samples of individual amphipods of E. verrucosus species collected in August 2020.
AzithromycinTetracyclineAcetaminophenIbuprofenAspirin
1−−−++
2−−−−−
3+++++
4+++++
5−−−−−
6−++−−
7−−−−−
8+++−−
9+++++
10+++++
11+++++
12+++++
13+++++
14+++++
15++++−
16+++++
Uncontaminated samples, %
Total3125253137
Contaminated samples, %
Total6975756963
“+” Presence of active of pharmaceutical ingredients; “−“ Absence of active of pharmaceutical ingredients.
Table 2. The presence of active pharmaceutical ingredients in samples of individual amphipods of E. verrucosus species collected in August 2020.
Table 2. The presence of active pharmaceutical ingredients in samples of individual amphipods of E. verrucosus species collected in August 2020.
AmikacinChlortetracyclineDoxycyclineOxytetracyclineDimetridazoleMetronidazoleSpiramycin
1++++++−
2−+++++−
3++++++−
4++++++−
5++++++−
6++++++−
7++++++−
8++++++−
9++++++−
10++++++−
11++++++−
12++++−++
13++++−++
14++++−+−
15++++−++
16++++−++
Uncontaminated samples, %
Total600031075
Contaminated samples, %
Total941001001006910025
“+” Presence of active of pharmaceutical ingredients; “−“ Absence of active of pharmaceutical ingredients.
Table 3. MRM transitions of active ingredients of drugs.
Table 3. MRM transitions of active ingredients of drugs.
Active Pharmaceutical
Ingredient		Precursor Ions (m/z)Product Ions (m/z)Reference
1Acetaminophen152.0110.0[68]
2Amikacin586.3425.2[69]
3Amoxicillin366.1114.1; 208[70]
4Ampicillin350.1192,1; 106.1[70]
5Apramycin540.3217.1[69]
6Aspirin179.0136.8[71]
7Azithromycin749.6591.6[72]
8Chlortetracycline479.1462.1[73]
9Clarithromycin748.5590.3; 158.0[74]
10Demeclocycline465.1430.1[73]
11Dimetridazole142.181.1; 96.1[70]
12Doxycycline445.1410.0[73]
13Erythromycin734.5158.0; 576.3[74]
14Florfenicol356.1185.1; 119.1[70]
15Gentamicin478.3157.1[69]
16Hygromycin B528.3352.1[69]
17Ibuprofen205.1161.1[75]
18Lincomycin407.2359.2; 126.0[74]
19Metronidazole172.1128.1; 82.1[70]
20Oxytetracycline461.1444.2[73]
21Spiramycin422.2100.9; 174.1[74]
22Sulfamethazine279.1186.1; 124.1[70]
23Sulfapyridine250.1184.1; 156.1[70]
24Tetracycline445.0410.0[73]
25Thiamphenicol353.9290.0; 184.9[70]
26Tylosin916.5772.1;174.0[74]
Table 4. HPLC separation program used for general screening.
Table 4. HPLC separation program used for general screening.
Time, minSolution A
100% Milli-Q Water, %		Solution B
100% Acetonitrile, %		Flow Rate, mL/min
0.59550.4
1.085150.4
6.020800.4
8.020800.4
9.09550.4
Table 5. HPLC separation program used to estimate ibuprofen concentration.
Table 5. HPLC separation program used to estimate ibuprofen concentration.
Time, minSolution A
0.1% Acetic Acid Solution, %		Solution B
100% Acetonitrile, %		Flow Rate, mL/min
0.560400.4
4.02980.4
6.02980.4
7.060400.4
7.560400.4
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Telnova, T.Y.; Morgunova, M.M.; Shashkina, S.S.; Vlasova, A.A.; Dmitrieva, M.E.; Shelkovnikova, V.N.; Malygina, E.V.; Imidoeva, N.A.; Belyshenko, A.Y.; Konovalov, A.S.; et al. Detection of Pharmaceutical Contamination in Amphipods of Lake Baikal by the HPLC-MS Method. Antibiotics 2024, 13, 738. https://doi.org/10.3390/antibiotics13080738

AMA Style

Telnova TY, Morgunova MM, Shashkina SS, Vlasova AA, Dmitrieva ME, Shelkovnikova VN, Malygina EV, Imidoeva NA, Belyshenko AY, Konovalov AS, et al. Detection of Pharmaceutical Contamination in Amphipods of Lake Baikal by the HPLC-MS Method. Antibiotics. 2024; 13(8):738. https://doi.org/10.3390/antibiotics13080738

Chicago/Turabian Style

Telnova, Tamara Y., Maria M. Morgunova, Sophie S. Shashkina, Anfisa A. Vlasova, Maria E. Dmitrieva, Victoria N. Shelkovnikova, Ekaterina V. Malygina, Natalia A. Imidoeva, Alexander Y. Belyshenko, Alexander S. Konovalov, and et al. 2024. "Detection of Pharmaceutical Contamination in Amphipods of Lake Baikal by the HPLC-MS Method" Antibiotics 13, no. 8: 738. https://doi.org/10.3390/antibiotics13080738

APA Style

Telnova, T. Y., Morgunova, M. M., Shashkina, S. S., Vlasova, A. A., Dmitrieva, M. E., Shelkovnikova, V. N., Malygina, E. V., Imidoeva, N. A., Belyshenko, A. Y., Konovalov, A. S., Misharina, E. A., & Axenov-Gribanov, D. V. (2024). Detection of Pharmaceutical Contamination in Amphipods of Lake Baikal by the HPLC-MS Method. Antibiotics, 13(8), 738. https://doi.org/10.3390/antibiotics13080738

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