A liquid chromatography-mass spectrometry method for the determination of the coccidiostats metronidazole, ronidazole, dimetridazole,
secnidazole, tinidazole and ipronidazole in feedstuff was developed. The 5-nitroimidazoles were extracted from animal feed
with a pH 2 phosphate buffer solution followed by a solid phase extraction procedure based on HLB cartridges. The liquid chromatographic
separation of the extracts was performed on a C18 bonded silica column applying a gradient of elution with pH 4.3 ammonium acetate buffer solution and acetonitrile. Quantification
for each 5-nitroimidazole was carried out monitoring its molecular ion [M + H]+ obtained by positive electrospray ionisation mode. A pool of feedstuffs was used to optimise and validate the method. Linearity,
quantification limit, intra-day and inter-day reproducibility and accuracy were estimated using this pool of feedstuffs spiked
with the drugs. For the confirmatory assay, several fragment ions from each 5-nitroimidazole were obtained and monitored.
The method was applied successfully to determine 5-nitroimidazoles in feedstuff at level of 0.05 mg kg−1. 相似文献
A capillary zone clectrophoresis method was developed for the determination of IMP and GIMP, commonly used as flavor enhancers in poultry feed, in a real sample of complex composition. A baseline separation of inosine 5′-monophosphate and guanosine 5′-monophosphate was achieved within 10 min and the other components in the sample did not interfere with the separation. Quantitative results obtained from pig feed samples are presented. The separation conditions and experimental reproducibility are also discussed. 相似文献
This paper studied the effect of pH and the viscosity of feed solution on the mass transfer in two different specifications of hydrophobic hollow fiber membrane contactors. Experimental results showed that the pH of the feed had a significant effect on the rate of mass transfer, the flux and the removal efficiency of easily ionized volatile compounds (VCs), such as ammonia. In unbuffered feed solutions, both the resistance of membrane and the resistance of feed side were affected by the pH of feed and both of them had contributions to the overall mass transfer. A model, , was proposed to predict the effect of pH and gave good agreement with the experimental data for the two contactors. The relationship between viscosities and the mass transfer coefficient could be described by . Based on our experiments, the change of the viscosities in the concentration range of ammonia from 50 to 10,000 mg l−1 caused about 3–4% variation of the mass transfer coefficients. Moreover, it may be more suitable to use the equilibrium concentrations of volatile species instead of the total concentrations of VCs to estimate mass transfer coefficients, removal efficiency and flux. Experimental results also revealed that the choice of the pH of feed might be one of the most crucial factors for removing easily ionized VCs, such as ammonia, from water and wastewater. 相似文献
Medical laboratories of the public sector as well as of the private sector on the island of Mauritius are preparing for accreditation. The clinical laboratory of the Central Health laboratory of the Ministry of Health and Quality of Life has undergone a pre-assessment by experts of the International Atomic Energy Agency (IAEA) through the aegis of a project targeted to members of the Africa Region. Several shortcomings were identified and respective corrective actions were recommended for implementation within a given time frame. In addition to ensuring the competence of the laboratory, accreditation has various positive aspects such as an increased awareness of the staff to quality and better training opportunities. The pre-assessment exercise has provided a gap analysis, which is an important aspect in the preparation towards accreditation. 相似文献
Recent developments in trapping efficiency inside ion trap mass spectrometer permitted to lower instrument detection limit (IDL). An IDL of 200 fg μl−1 injected with a signal-to-noise ratio of 5:1 for tetrachlorodibenzo-p-dioxin (TCDD) was obtained by gas chromatography coupled to a quadrupole ion storage mass spectrometer in tandem mode (GC/MS/MS). Coupling large volume programmable temperature vaporizer (PTV-LV) injection to GC/MS/MS provides an alternative and complementary method to classical splitless-GC injection connected to high-resolution mass spectrometry (splitless-GC/HRMS) method for dioxin monitoring in food and feed.
An injection volume of 10 μl was found to be the best compromise between the sensitivity requirements and the robustness required for a high throughput method. PTV-LV-GC/MS/MS and Splitless-GC/HRMS were compared by performing analysis on five different matrices such as beef fat, yolk eggs, milk powder, animal feed and serum samples covering a concentration range of two orders of magnitude (i.e. 0.2–25 ng WHO-TEQ kg−1). An analysis of variance (ANOVA) was carried out. Fisher tests pointed out that the method effect for all the 2,3,7,8 congeners was not significant, indicating that the null hypothesis (H0: μ1=μ2=…=μn) was not rejected. Moreover, the interaction effects between methods and matrices were not significant for most of the 2,3,7,8 congeners. However, three congeners (2,3,7,8-TCDF; 1,2,3,4,7,8-HxCDD and 1,2,3,4,6,7,8-HpCDD) were characterized by P-values lower than the significance level (=0.05). In toxic equivalence (TEQ), the study showed that no significant bias was observed between the two methods. Consequently, PTV-LV-GC/MS/MS is an attractive technique and can be used as a cost effective complementary method to HRMS for dioxin levels monitoring in food and feed. 相似文献
Zilpaterol, (±)‐trans‐4,5,6,7‐tetrahydro‐7‐hydroxy‐6‐(isopropylamino) imidazo [4,5,1‐jk]‐[1]benzazepin‐2(1H)‐one, is an adrenergic agonist drug licensed in Mexico and South Africa as feed additive for cattle at slaughter age. In contrast, the EU legislative framework prohibits the use of beta‐agonists as growth promoters to produce lean meat. In this study, the compound was quantified as its TMS derivative both by gas chromatography‐mass spectrometry (GC‐MS) with a quadrupole detector (QUADR) and by GC‐MS/MS with an ion trap detector (ITD), in Electron Impact (EI) ionization. Subsequently, an extraction and clean‐up procedure for the identification of Zilpaterol in commercial feeds was set up. Different extraction solvents and matrices were considered for their influence on Zilpaterol yield. The analytical method led to good recoveries and limits of detection and quantification in feeds well below the 5–20 μg/g dose proposed for animal nutrition. 相似文献
Labeled RNAs are invaluable probes for investigation of RNA function and localization. However, mRNA labeling remains challenging. Here, we developed an improved method for 3′-end labeling of in vitro transcribed RNAs. We synthesized novel adenosine 3′,5′-bisphosphate analogues modified at the N6 or C2 position of adenosine with an azide-containing linker, fluorescent label, or biotin and assessed these constructs as substrates for RNA labeling directly by T4 ligase or via postenzymatic strain-promoted alkyne-azide cycloaddition (SPAAC). All analogues were substrates for T4 RNA ligase. Analogues containing bulky fluorescent labels or biotin showed better overall labeling yields than postenzymatic SPAAC. We successfully labeled uncapped RNAs, NAD-capped RNAs, and 5′-fluorescently labeled m7Gp3Am-capped mRNAs. The obtained highly homogenous dually labeled mRNA was translationally active and enabled fluorescence-based monitoring of decapping. This method will facilitate the use of various functionalized mRNA-based probes. 相似文献