Comparison of microbial receptor assay and liquid chromatography for determination of penicillin G and amoxicillin in milk powder

A microbial receptor assay (Charm II Tablet Beta-Lactam Test) and liquid chromatography (LC) were compared for determination of penicillin G (PG) and amoxicillin (AMOX) in reconstituted milk powder. Nonfat dry milk and whole dry milk were reconstituted (10%, w/v) to concentrations of 0, 2.5, 5, 7.5, and 10 ppb PG; nonfat dry milk was reconstituted (10%, w/v) to 0, 7.5, 10, and 15 ppb AMOX. Reconstituted samples were analyzed blindly by each method. Concentrations determined by both methods demonstrated good agreement. A significant difference between methods (p < or = 0.05) was observed only for 7.5 ppb PG in defatted dry milk. Significant differences were not observed between known concentrations and concentrations determined by the Charm II assay for PG or AMOX in defatted dry milk and PG in whole dry milk. Results by LC showed significant differences (p < 0.05) between known and measured concentrations at 10 ppb PG in both milks and 0 ppb AMOX in defatted dry milk. These results suggest that both the microbial receptor assay and LC may be useful for determination of PG and AMOX near safe level and tolerance, respectively, in reconstituted milk powder.     

Application of centrifugal vacuum concentrators in residue analysis

Summary Centrifugal vacuum concentrators can be applied in residue analysis successfully: They prevent the samples from bumping and foaming. Even methanol/water- or acetonitrile/water-mixtures as extracts from food or other samples can be concentrated without separation of water prior to the evaporation process. Sulfonamides and other drugs can be concentrated with 100% recovery. Extracts with some light-sensitive substances (nitrofuranes) were evaporated without losses, as well as some hydrolysis-sensitive substances (penicillins) solved in water, whereas tetracyclines decompose in aqueous solution considerably. For more volatile substances (such as organochlorine pesticides or polychlorinated biphenyls) centrifugal vacuum concentrators can be used for preconcentration e.g. of the gelchromatographic eluate. Further, centrifugal vacuum concentrators can automate the evaporation process. In comparison to rotary evaporators, they save time for the laboratory staff when running series of 4 or more samples. It is very important to supply permanently sufficient energy for the evaporation process, especially when concentrating volumes of 10 ml or more. If the only heated part is the wall of the centrifuge, after couple of minutes the samples cool down to very low temperatures, and the evaporation process slows down. A more efficient way to supply evaporation energy is by means of IR radiation. A very modern device offers an electronically controlled IR radiation by means of temperature control on the centrifugal tubes. This in combination with vapour pressure control ensures an optimal control of the most important factors of the evaporation process.     

High-performance liquid chromatographic determination of penicillin G, penicillin V and cloxacillin in beef and pork tissues.

The objective was to develop confirmatory high-performance liquid chromatographic methods for penicillin residues in animal tissues with detection limits of less than or equal to 10 ng/g. A previously described procedure was modified by using a larger sample size and isocratic analysis. Tissues (15 g) were blended with 45 ml of water and 20 ml of homogenate were mixed with 40 ml acetonitrile and filtered. The filtrate (30 ml) was mixed with 10 ml of 0.2 M H3PO4 and extracted with methylene chloride. The combined methylene chloride layers were mixed with acetonitrile and hexane, washed with two 4-ml portions of water and then extracted with four 1-ml portions of 0.01 M phosphate buffer (pH 7). The combined buffer extracts were concentrated to 1 ml under reduced pressure. Analysis was isocratic during 0.01 M phosphate buffer (pH 7)-acetonitrile with proportions 85:15 (penicillin G), 82:18 (penicillin V) or 78:22 (cloxacillin). A polystyrene-divinylbenzene copolymer column, 150 x 4.6 mm I.D. (Polymer Labs. PLRP-S), was used with a flow-rate of 1 ml/min and detection at 210 nm. The presence of penicillins was confirmed by treating a duplicate sample with penicillinase. Recoveries were greater than 90% in most instances. Detection limits were 5 ng/g in muscle and higher in liver and kidney. The procedure is a simple and sensitive method for confirming the presence of penicillins in animal tissues.     

Determination of tetracycline antibiotics in tissues and blood serum of cattle and swine by high-performance liquid chromatography

Tissue homogenates and blood serum were acidified with hydrochloric acid and deproteinized with acetonitrile. Tetracyclines were partitioned into water and concentrated by solid-phase absorption on the analytical column form 0.01 M phosphoric acid-methanol (80:20). Tetracyclines were eluted with an acetonitrile gradient. An all-organic polymeric column (Polymer Labs. PLRP-S) was used. Similar results were obtained on a bonded reversed-phase column after addition of tetramethyl-ammonium chloride to the mobile phase. Recoveries were near 100% from blood serum, 83-94% from muscle, and 80-100% from liver and kidney with sensitivities of 0.1 ppm or less for muscle and blood serum.     

Spectroscopic assignments of the excited B-mesons

The European Physical Journal A - We report on the development and characterization of the first radioactive boron beams produced by the isotope mass separation online (ISOL) technique at...     

Confirmatory test results on milk from commercial sources that tested positive by beta-lactam antibiotics screening tests.

Fifty-four milk samples from commercial sources that tested positive for beta-lactam antibiotics were analyzed by a multiresidue liquid chromatographic (LC) procedure based on LC fractionation. Penicillin G and cephapirin were the beta-lactam antibiotics found most frequently. Some samples did not contain detectable beta-lactam antibiotics. In a few, the presence of a beta-lactam antibiotic was suspected because certain LC fractions tested positive for antimicrobial activity, which was no longer present in a replicate treated with beta-lactamase. However, the unknowns could not be identified by LC analysis.