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1.
Antimicrob Agents Chemother ; 42(9): 2456-8, 1998 Sep.
Article in English | MEDLINE | ID: mdl-9736585

ABSTRACT

Several known mammalian ribonucleotide reductase inhibitors featuring a polyhydroxyphenyl and/or hydroxamate moiety as the active group were screened for potency in inhibiting growth of the malaria parasite Plasmodium falciparum. Compounds containing a 2,3- or 3,4-dihydroxyphenyl group as well as benzohydroxamate appear to be the most effective inhibitors of the malaria parasite.


Subject(s)
Antimalarials/pharmacology , Hydroxamic Acids/pharmacology , Ribonucleotide Reductases/antagonists & inhibitors , Animals , Hydroxyurea/pharmacology , Plasmodium falciparum/drug effects , Structure-Activity Relationship
2.
J AOAC Int ; 78(2): 483-91, 1995.
Article in English | MEDLINE | ID: mdl-7756864

ABSTRACT

A four-laboratory validation study of a method for the quantitation and confirmation of low part-per-billion levels of chloramphenicol extracted from veal calf urine was done. With this method, chloramphenicol, derivatized to the bis(trimethylsilyl)ether, was quantitated by gas chromatography with electron capture detection (GC-ECD) and confirmed by selected-ion monitoring in a negative ion chemical ionization gas chromatograph-mass spectrometer (GC-NICI-MS). Four analysts from 4 laboratories participated in the portion of the study devoted to chloramphenicol quantitation. Every analyst analyzed 5 sets, one set per day, on 5 different days. Each set included 6 samples consisting of a blank, 2 fortified samples, 2 incurred urine samples, and one duplicate. Thus, each analyst worked on a total of 30 samples. Chloramphenicol concentrations ranged from 0 to 9.7 ppb. All data were reported to 0.1 ppb. Coefficients of variation for distribution, CVd, ranged from 8.82 to 14.14% and for precision, CVr, ranged from 9.15 to 14.80%. Three analysts from 3 laboratories also participated in the confirmatory portion of the study, which was carried out to test whether the NICI-MS method developed earlier for higher concentrations of chloramphenicol and for an extract of muscle tissue could be applied to lower levels of chloramphenicol and to an extract prepared from urine. The extracts of 10 of the 30 samples were designated for confirmation only, but were obtained by the same procedure as extracts used for the quantitation part of the study.(ABSTRACT TRUNCATED AT 250 WORDS)


Subject(s)
Cattle/urine , Chloramphenicol/urine , Chromatography, Gas/methods , Animals , Mass Spectrometry , Reproducibility of Results , Temperature
3.
J AOAC Int ; 77(4): 917-24, 1994.
Article in English | MEDLINE | ID: mdl-8069123

ABSTRACT

A gas chromatographic/mass spectrometric procedure is described for the quantitation and confirmation of clenbuterol residues from cattle, sheep, and swine tissues. After liquid-liquid extraction and derivatization with phosgene in an aqueous pH 10.1 buffer, the cyclic oxazolidone derivative is quantitated with a clenbuterol analogue as internal standard (NAB-760 Cl). Confirmation is accomplished by comparison of ion ratios with those of a pure synthesized standard of clenbuterol oxazolidin-3-one obtained by selected ion monitoring, electron ionization gas chromatography/mass spectrometry on a benchtop instrument. Statistical information based on a series of standard curves for fortified tissues is included to describe method performance. Ion ratio variations were under 15%, and coefficients of variation for spiked tissue standard curves were above 0.997. Recoveries averaged 87.1 +/- 6.6% for liver tissues across all 3 species and 67.1 +/- 3.8% for muscle tissue across all 3 species.


Subject(s)
Clenbuterol/analysis , Gas Chromatography-Mass Spectrometry/methods , Liver/chemistry , Muscles/chemistry , Animals , Cattle , Sheep , Swine
4.
J AOAC Int ; 77(3): 570-6, 1994.
Article in English | MEDLINE | ID: mdl-8012202

ABSTRACT

A gas chromatographic (GC) procedure for the quantitation and GC/negative ion chemical ionization mass spectrometric (NICIMS) confirmation of chloramphenicol in calf muscle tissue was the subject of a validation study. Five analysts representing 5 laboratories in 4 countries participated in the quantitative method and analyzed 7 randomly numbered blind triplicates at 4 fortified and 3 incurred tissue concentrations on 3 separate days. The chloramphenicol concentrations ranged from 0 to 2.5 ppb. All data were reported to 3 significant figures. The coefficients of variation were 9.5-28.7% for repeatability and 14.6-38% over the study range for reproducibility. NICIMS data representing 3 laboratories in 3 countries successfully confirmed chloramphenicol in samples at 0.6 ppb or greater with no false positives in blank tissues.


Subject(s)
Cattle , Chloramphenicol/analysis , Chromatography, Gas/statistics & numerical data , Gas Chromatography-Mass Spectrometry/statistics & numerical data , Muscles/chemistry , Animals , Reproducibility of Results
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