A sensitive and robust confirmatory method for determination of steroid esters in blood serum is essential for reliable monitoring of possible illegal use of steroid hormones as growth promoters in meat production. A previously used sample preparation methodology was improved. The procedure consists of protein precipitation and removal of phospholipids by dispersive SPE Supel™ QuE Z-Sep (Sigma-Aldrich) followed by clean-up on alumina column and LC-MS/MS measurement. The modified method has been validated according to Commission Decision 2002/657/EC. Validation parameters for determination of six testosterone esters and five nortestosterone esters in bovine and porcine blood serum are presented in this article. Decision limits for all analytes were observed in the range 10-20 pg mL-1. The method described is considerably robust for bovine and porcine serum analyses and can be applied both for screening and confirmatory determination in routine residue monitoring.
Monitoring of steroid esters in blood serum is desirable in order to detect the possible illegal use of natural hormones as growth promoters. A method for the determination of testosterone propionate, testosterone benzoate, testosterone isocaproate, testosterone decanoate and estradiol benzoate in bovine and porcine blood serum was developed. The procedure consists of protein precipitation and removal of phospholipids using a HybridSPE®-Phospholipid column followed by clean-up on a hydrophilic modified styrene polymer Supel(TM)-Select HLB column and LC-MS/MS measurement. The method was validated according to Commission Decision 2002/657/EC. Decision limits for all analytes were observed in the range 5-30 pg ml(-)(1). The method was shown to be robust for bovine and porcine serum analyses and can be applied for both screening and confirmatory determination in routine residue monitoring.
- MeSH
- chemická precipitace MeSH
- chromatografie kapalinová normy MeSH
- dihydrotestosteron analogy a deriváty krev MeSH
- estradiol analogy a deriváty krev MeSH
- fosfolipidy izolace a purifikace MeSH
- krevní proteiny chemie MeSH
- limita detekce MeSH
- prasata MeSH
- skot MeSH
- směrnice jako téma MeSH
- tandemová hmotnostní spektrometrie normy MeSH
- testosteron analogy a deriváty krev MeSH
- testosteronpropionát krev MeSH
- zvířata MeSH
- Check Tag
- skot MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články 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.
- 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
To investigate potential residues in tissues arising from naturally occurring low levels of chloramphenicol in plant material, feeding studies were conducted with chickens. A common chicken feed was prepared containing 0, 10, 50 and 200 μg kg(-1) chloramphenicol and levels were confirmed by LC-MS/MS. Four separate groups of broiler chickens, eight animals in each group, were fed all their 35-day life with this contaminated feed. They were allowed ad libitum access to this feed and fresh water. After slaughtering the chickens, the residues in muscle and liver tissues were determined using GC/MS-NCI method. No residues were detected in tissues of animals from groups fed with feed containing 0, 10 or 50 µg kg(-1). Low chloramphenicol residual concentrations were observed in a few of the muscle samples obtained from the group of chickens fed with feed containing chloramphenicol in added concentration 200 µg kg(-1). No residues were detected in the remaining samples of this group. These results indicate that when residues of chloramphenicol are detected it is in all probability through illegal use.
- MeSH
- antibakteriální látky aplikace a dávkování analýza MeSH
- chloramfenikol aplikace a dávkování analýza MeSH
- chromatografie kapalinová MeSH
- játra chemie MeSH
- kontaminace potravin analýza MeSH
- kontrola léčiv a omamných látek zákonodárství a právo MeSH
- krmivo pro zvířata analýza MeSH
- kur domácí MeSH
- lidé MeSH
- limita detekce MeSH
- maso analýza MeSH
- svaly chemie MeSH
- tandemová hmotnostní spektrometrie MeSH
- veterinární léky aplikace a dávkování analýza MeSH
- zvířata MeSH
- Check Tag
- lidé MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
A method for the determination of residues of six steroids with gestagenic action (altrenogest, medroxyprogesterone acetate, megestrol acetate, melengestrol acetate, acetoxyprogesterone and chlormadinone acetate) in animal fat tissue was developed. The procedure consists of methanol extraction, clean-up on an alumina column and LC-MS/MS measurement. The method has been validated according to Decision 2002/657/EC. Decision limits for all analytes were observed within the range from 0.3 to 1.7 ng g(-1), and recoveries were between 80% and 105%. The method is robust and can be applied for both screening and confirmatory analyses in routine residue monitoring.
A method for determination of low concentrations of chloramphenicol in urine, feed water, milk and honey was developed. A comparison was carried out between a routinely used analytical method based on solid phase extraction (SPE-C18) for cleaning the extract and the new procedure for the sample preparation using columns based on the molecular imprinted polymers (MIP) principle. The extracts obtained from the MIP clean-up procedure were clean enough for chromatografic analyses. Confirmatory analyses were conducted using GC/MS-NCI after derivatisation (silylation). The described method was fully validated according to CD 2002/657/EC. This method is considerably robust and allows very dirty samples to be processed. The described MIP procedure is very simple and low-time-consuming, and provides high throughput of the samples examined. This could be used for routine screening and confirmatory analyses as well.
- MeSH
- antibakteriální látky moč MeSH
- chloramfenikol moč MeSH
- chromatografie metody přístrojové vybavení MeSH
- krmivo pro zvířata analýza MeSH
- med analýza MeSH
- mléko chemie MeSH
- molekulový imprinting MeSH
- polymery chemie MeSH
- prasata MeSH
- skot MeSH
- voda analýza MeSH
- zvířata MeSH
- Check Tag
- skot MeSH
- zvířata MeSH
- Publikační typ
- hodnotící studie MeSH
