The growing consumption of pharmaceuticals in the human population and the insufficient efficiency of their elimination in waste water has a long-term negative impact on the environment of aquatic ecosystems, including the organisms that inhabit them. A significant contributor is the consumption of anti-depressants from the SSRI group, which corresponds to their increasing concentration in the environment. The aim of this work was to determine if antidepressant sertraline is able to be stored in fish organisms and to evaluate the content of residues in various body tissues. Rainbow trout (Oncorhynchuss mykkis) was selected as the test organism and was artificially exposed to the antidepressant for 1 month (concentrations 0; 4.2; 44 and 400 ng.g-1 sertraline in the feed). Liver, kidney, brain and muscle tissue biopsies samples were taken for analysis. Detection was performed using an Accela 1250 LC pump and an Accela autosampler coupled with a high-performance mass analyzer with a heated electrospray ionization source Q-Exactive Orbitrap, operating in positive ionization mode and in PRM mode (m/z 306.08108->275.03888 and 309.009991->275.03888 for sertraline and internal standard, respectively). The limit of quantification of the method was 0.1 ng.g-1 of sertraline and the calibration curve showed a good linearity up to 20 ng.g-1. From the collected data, amount of residues was found in the liver, kidney and brain. In contrast, the incidence of residues in muscle tissue was not detected in all groups, which is favorable from the point of view of fish meat consumption, by humans.
- MeSH
- chemické látky znečišťující vodu analýza MeSH
- hmotnostní spektrometrie s elektrosprejovou ionizací * MeSH
- obsah radioaktivních látek v organizmu MeSH
- Oncorhynchus mykiss metabolismus MeSH
- rezidua léčiv analýza MeSH
- selektivní inhibitory zpětného vychytávání serotoninu analýza MeSH
- sertralin analýza MeSH
- tandemová hmotnostní spektrometrie * MeSH
- tkáňová distribuce MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- chemické látky znečišťující vodu MeSH
- selektivní inhibitory zpětného vychytávání serotoninu MeSH
- sertralin MeSH
This paper presents the results from a residue study conducted on a statistically representative number of chicken broilers that were individually orally treated with the selected nitroimidazoles (metronidazole, ornidazole and ipronidazole) in an appropriate amount close to the theoretical therapeutic dose. A mutual persistence comparison of the monitored analytes in feathers, serum, muscle and shanks was performed and attention was also paid to selected metabolites (hydroxymetronidazole and hydroxyipronidazole). An analytical LC/MS/MS method using SupelMIP SPE nitroimidazoles cartridges was developed for the determination of nitroimidazoles residues in poultry feathers, serum, muscle and shanks and the method was validated according to Commission Decision 2002/657/EC. High concentrations of nitroimidazoles residues in feathers were observed 19 days after the broilers' treatment unlike the muscle and serum samples, where nitroimidazoles depletion was significantly faster (residue concentrations were below detection limits in 5 days in muscle and in 12 days in serum). Shanks (chicken claws) also proved to be a very useful matrix for the detection of nitroimidazoles drugs misuse due to the longer persistence of these drugs residues and their metabolites in this matrix (determinable concentrations were observed 19 days after the broilers' last treatment). Feathers and shanks appear to be suitable matrixes for the screening of various nitroimidazoles in poultry because long-term persistence of residues enables reliable detection of the illegal use of nitroimidazoles compounds in official checks.
- Klíčová slova
- LC/MS/MS, Nitroimidazoles, chicken, feathers, residual study, shanks,
- MeSH
- aplikace orální MeSH
- kur domácí * MeSH
- nitroimidazoly aplikace a dávkování analýza MeSH
- peří chemie MeSH
- rezidua léčiv analýza MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- srovnávací studie MeSH
- Názvy látek
- nitroimidazoly MeSH
A simple, robust and effective extraction procedure for the determination of 74 pharmaceuticals in different fish tissues by ultrasensitive high performance liquid chromatography with electrospray high resolution product scan (HPLC-ESI-HRPS) was developed and validated. Different extraction solvent mixtures were tested to achieve the highest recoveries of the selected analytes, to minimize the influence of a complex matrix and to reduce the total analysis time as well as cost of analysis. A mixture of acetonitrile + isopropanol (3:1 v/v) acidified with 0.1% formic acid was the best extraction solvent among the five solvents tested for most of the tissues with the exception of plasma samples, where only acidified acetonitrile exhibited the best performance. The developed method was validated at three concentration levels (5, 20 and 50 ng g-1) in five different fish tissues (liver, kidney, brain, muscle and plasma). Most of the target analytes were extracted with a recovery between 60 and 130%. Very low limits of quantification (LOQs) were obtained for the majority of the pharmaceuticals in all of the studied matrices. The developed analytical method was successfully applied for the analysis of common carp (Cyprinus carpio) originating from the waste water effluent-dominated pond Cezarka (Czech Republic). The results confirmed the importance of multi-tissue analysis to obtain complex information on the distribution of pharmaceuticals in fish.
- Klíčová slova
- Fish tissues, Micropollutants, Multicomponent analysis, Sample pre-treatment,
- MeSH
- 2-propanol chemie MeSH
- acetonitrily chemie MeSH
- chemická frakcionace metody MeSH
- kapři * MeSH
- monitorování životního prostředí MeSH
- reprodukovatelnost výsledků MeSH
- rezidua léčiv analýza izolace a purifikace MeSH
- společenstvo * MeSH
- vysokoúčinná kapalinová chromatografie MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- 2-propanol MeSH
- acetonitrile MeSH Prohlížeč
- acetonitrily MeSH
One-day-old chickens were individually orally treated with chloramphenicol at a dose of 100 mg per kg of body weight per day for three consecutive days. After the final treatment, the groups of six birds were sacrificed in seven-day intervals up to 42 days. The muscle tissue collected from the breasts and legs of each bird was individually examined for the presence of chloramphenicol residues using a GC/MS-NCI analytical method, which was validated according to Commission Decision 2002/657/EC. The decision limit (CCα) obtained for the method was 0.05 ng g-1. The results showed a rapid decrease of chloramphenicol concentration in the muscle tissue after termination of the treatment, but also showed a relatively long persistence of low residue concentrations. Levels of chloramphenicol in muscle tissue averaged 64 ng g-1 seven days after the final treatment and fell to 0.21 ng g-1 after 35 days. All animals tested on the 35th day after the final treatment showed detectable chloramphenicol concentrations above the decision limit of the method used. No residues were detected in the animal tissues 42 days after the end of the treatment.
- Klíčová slova
- Chloramphenicol residues, GC/MS-NCI, chicken,
- MeSH
- antibakteriální látky aplikace a dávkování analýza MeSH
- chloramfenikol aplikace a dávkování analýza MeSH
- chromatografie kapalinová MeSH
- kontaminace potravin analýza MeSH
- kur domácí MeSH
- lidé MeSH
- limita detekce MeSH
- maso analýza MeSH
- rezidua léčiv analýza MeSH
- směrnice jako téma MeSH
- svaly chemie MeSH
- tandemová hmotnostní spektrometrie MeSH
- tělesná hmotnost MeSH
- veterinární léky aplikace a dávkování analýza MeSH
- zvířata MeSH
- Check Tag
- lidé MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- antibakteriální látky MeSH
- chloramfenikol MeSH
- veterinární léky MeSH
An enzyme-linked immunosorbent assay (ELISA) method is described for the semi-quantitative determination of semicarbazide (SEM), the marker residue for the banned nitrofuran drug, nitrofurazone, in chicken eggs. The sample homogenate is subjected to acid hydrolysis and derivatisation with o-nitrobenzaldehyde, followed by ethyl acetate/hexane extraction and detection by ELISA. The ELISA procedure has been validated using 0.3, 1.0 and 3 microg kg(-1) of SEM in fortified samples. Detection capability (CC(ss)) was based on the acceptance of 5% false compliant results for a given concentration level according to Commission Decision 2002/657/EC and was determined to be 0.3 microg kg(-1) with a respective limit of detection of 0.13 microg kg(-1). A validated LC-MS/MS method was used for the analysis of incurred egg samples and the results compared with ELISA. A good correlation between the results obtained from ELISA and LC-MS/MS within the concentration range 0.12-20.3 microg kg(-1) was observed in samples collected from chickens fed with a medicated ration of nitrofurazone (r = 0.992, n = 14). Validated ELISA enabled reliable monitoring of SEM levels in eggs collected from incurred chickens over a 90-day period.
- MeSH
- chromatografie kapalinová metody MeSH
- ELISA metody MeSH
- hmotnostní spektrometrie metody MeSH
- karcinogeny analýza MeSH
- kontaminace potravin analýza MeSH
- kontrola léčiv a omamných látek MeSH
- kur domácí MeSH
- nitrofurazon MeSH
- rezidua léčiv analýza MeSH
- semikarbazidy analýza MeSH
- vejce analýza MeSH
- zvířata MeSH
- Check Tag
- ženské pohlaví MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- validační studie MeSH
- Názvy látek
- carbamylhydrazine MeSH Prohlížeč
- karcinogeny MeSH
- nitrofurazon MeSH
- semikarbazidy MeSH
HPLC method with solid phase extraction, and microbiological agar diffusion tests for determination of oxytetracycline (OTC), tetracycline (TC) and chlortetracycline (CTC) in bones, mechanically separated beef and bones were developed. Both mechanically separated bones and bovine flat bones showed the highest yield of tetracyclines by HPLC method. Among tetracyclines, the highest yield was determined in chlortetracycline. The strains of Bacillus subtilis (PH 6.0) and B. stearothermophilus showed the highest sensitivity to the presence of tetracyclines.
- MeSH
- bakteriologické techniky MeSH
- biotest MeSH
- kosti a kostní tkáň chemie MeSH
- masný průmysl MeSH
- maso analýza MeSH
- rezidua léčiv analýza MeSH
- skot MeSH
- tetracyklin analýza MeSH
- zvířata MeSH
- Check Tag
- skot MeSH
- zvířata MeSH
- Publikační typ
- anglický abstrakt MeSH
- časopisecké články MeSH
- Názvy látek
- tetracyklin MeSH
The objective of this study was to determine the oxytetracycline residues in milk from cows with clinical mastitis dosed with two extra-label routes of oxytetracycline administration not only during antibiotic's treatment (5 days), but also six days after treatment by use of a liquid chromatography method of testing with a detection limit of 20 ppb. Both groups of animals were treated once daily for five milkings at 24-hour intervals following morning milkings. Composite milk samples (equal volumes of foremilk from each quarter) were collected during morning and afternoon milkings, mixed together (1:1), and stored until analyzed. Milk samples were analyzed just before the first treatment (0 hour) and ten times at 24-hour intervals. Residue studies in milk cows indicate that oxytetracycline passes into milk. Residues in milk were higher for the cows receiving oxytetracycline by intramammary route (Tab. I) than for the cows receiving oxytetracycline intramuscularly (Tab. II). The highest mean data were 195.68 mg/kg after intramammary infusion (Fig. 2) and 2.74 mg/kg after intramuscular injection (Fig. 3) on the 5th day of the treatment beginning. The analysis data showed that oxytetracycline persisted in milk for as long as two days after both treatments at the concentration 0.03 mg/kg versus 0.02 mg/kg, respectively. No residues were detected in milk of any animal from the 4th day of the cessation of the therapy (Fig. 1) as detected by the HPLC method.
- MeSH
- antibakteriální látky analýza terapeutické užití MeSH
- laktace metabolismus MeSH
- mastitida skotu farmakoterapie metabolismus MeSH
- mléko chemie MeSH
- oxytetracyklin analýza terapeutické užití MeSH
- rezidua léčiv analýza MeSH
- skot MeSH
- zvířata MeSH
- Check Tag
- skot MeSH
- ženské pohlaví MeSH
- zvířata MeSH
- Publikační typ
- anglický abstrakt MeSH
- časopisecké články MeSH
- Názvy látek
- antibakteriální látky MeSH
- oxytetracyklin MeSH
Residual antibiotics in milk were identified by high-voltage electrophoresis in 1% agarose gel and bioautographic detection. The test strain Bacillus subtilis BGA was used for the detection, pH of the culture medium was 8.0. An electrophoretic identification map of 13 selected antibiotics has been set up and the following minimal inhibition concentrations (MIC), expressed in microgram per 1 g, have been established: benzylpenicillin 0.06; ampicillin 0.25; streptomycin 0.5; dihydrostreptomycin 0.2; spectinomycin 40; gentamycin 0.06; neomycin 0.15; oxytetracycline 5; tetracycline 2.5; chlortetracycline 1; erythromycin 0.01; tylosin 1; chloramphenicol 20. The established values of MIC were compared with the Maximum Residue Limits (MRL) as defined currently in the legislation of the European Union. The condensation of samples by freeze-drying increased the sensitivity of the method which was used for the identification of residual antibiotics detected by microbiological screening techniques in milk.
- MeSH
- antibakteriální látky analýza MeSH
- elektroforéza MeSH
- mléko chemie MeSH
- rezidua léčiv analýza MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- antibakteriální látky MeSH
Difficulties with harmonization of analytical procedures and consequently poor comparability of generated data represent in the Czech Republic the main reason for the delay in issuing of updated legislation for polychlorobiphenyls (PCBs) in foodstuffs. This study draws attention to possible errors (overestimations) that can occur during routine determination of these residues in the fat portion of biotic matrices. We demonstrate the gas chromatographic (GC) conditions under which interfering contaminants such as phthalates and/or chlorinated pesticides can be separated from analytes. Discussion is focused on the advantages and drawbacks of GC with an electron capture detector, GC mass spectrometry and GC with an atomic emission detector. Various approaches used for calculation of PCBs contents are compared.
- MeSH
- chromatografie plynová MeSH
- kontaminace potravin analýza MeSH
- krmivo pro zvířata MeSH
- mléko chemie MeSH
- monitorování životního prostředí MeSH
- mutageny analýza MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí MeSH
- polychlorované bifenyly analýza MeSH
- reprodukovatelnost výsledků MeSH
- rezidua léčiv analýza MeSH
- skot MeSH
- tuková tkáň chemie MeSH
- zvířata MeSH
- Check Tag
- skot MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- Geografické názvy
- Česká republika MeSH
- Názvy látek
- Delor 106 MeSH Prohlížeč
- mutageny MeSH
- polychlorované bifenyly MeSH
Negative detection of residues of inhibitory substances has become one of the standard quality traits of raw milk also in the Czech Republic. Hence a requirement appeared in 1991 to evaluate the usability of two commercially produced microtitration tests for this purpose. The tests of BR-TEST (Enterotox) and INTEST (Mlékárenský průmysl) were performed in weekly intervals for the time longer by a week than is the declared expiration, that means seven replications in BR-TEST and five replications in INTEST. Compact and stripped microplates (STRIPS) designated BR-TEST "AS", BR-TEST 12x8 "AS" and INTEST C-96 type and INTEST 0-96/6x16 were used for the tests. The principle of inhibition demonstration in the concentration series of selected drugs was applied. The drugs were chosen with respect to the frequency of their use for clinical treatments in the CR. Tab. II shows the used drugs and concentration series. The following parameters were tested: detection limits, reproducibility, effect of milk preservation, and the declared expiration. Tab. III shows detection limits. It is apparent the BR-TEST detection responses to streptomycin and chloramphenicol were lower in BR-TEST than in INTEST in our experiments. The responses to penicillin, oxacillin and oxytetracycline were lower in some cases, and equal in other ones. On the other hand, the INTEST detection response to sulfadimidin was markedly lower in comparison with BR-TEST. Tab. IV summarizes the range of detection limits in milk with Heeschen's reagent. In our experiments the detection response of BR-TEST to the tested chemotherapeutics was lower in some cases, in other cases it was the same as in INTEST.(ABSTRACT TRUNCATED AT 250 WORDS)
- MeSH
- analýza potravin metody MeSH
- kontaminace potravin * MeSH
- mléko chemie MeSH
- rezidua léčiv analýza MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- anglický abstrakt MeSH
- časopisecké články MeSH
