Modified determination of dihydrostreptomycin in kidney, muscle and milk by HPLC†

Abbasi, Hasan; Hellenäs, Karl-Erik

doi:10.1039/a804910f

Cited by 24 publications

(13 citation statements)

References 5 publications

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“…These values indicate that the extraction procedure described for sample preparation was effective, and the developed method had acceptable precision. The findings of the present study were consistent with those reported by Edder et al (1999) (81%), and were slightly higher than those reported by for DHS in muscle by Abbasi and Hellenäs (1998) …”

Section: Methods Validationsupporting

confidence: 86%

“…The complexity of food samples makes it necessary to perform sample clean-up by solid-phase extraction (SPE) prior to LC-fluorescence analysis (Gerhardt et al, 1994;Abbasi and Hellenäs, 1998). High-performance liquid chromatography (HPLC), gas chromatography-mass spectroscopy (GC-MS) and liquid chromatography-mass spectroscopy (LC-MS) have been described for confirmatory analysis (Gerhardt et al, 1994;Abbasi and Hellenäs, 1998;Stead, 2000). Confirmatory methods are not considered as alternatives because they are highly specific and require sophisticated equipment and skilled laboratory personnel.…”

Section: Introductionmentioning

confidence: 99%

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Monitoring of streptomycin and dihydrostreptomycin residual levels in porcine meat press juice and muscle via solid‐phase fluorescence immunoassay and confirmatory analysis by liquid chromatography after post‐column derivatization

Pyun

El‐Aty

Hashim

et al. 2007

Biomedical Chromatography

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A solid-phase fluorescence immunoassay (SPFIA) that was primarily developed for detection of antibiotic residues in milk was qualitatively applied for the pre-screening of the residues of aminoglycoside antibiotics, streptomycin and dihydrostreptomycin, in meat press juice. The confirmation of both analytes was performed using a validated method of highperformance liquid chromatography with post-column derivatization. The analytical performance was demonstrated by the analysis of pork meat samples spiked at three concentration levels, ranging from 0.25 to 2.5 ppm for each analyte. In general, the recoveries ranged from 80.4 to 81.5% and from 79.6 to 84.4% for streptomycin and dihydrostreptomycin, respectively, with relative standard deviations lower than 6%. The limits of detection were 0.1 and 0.15 ppm for streptomycin and dihydrostreptomycin, respectively, and the limits of quantification of 0.35 and 0.5 ppm are below the maximum residue limits of Codex, the European Union, and the Korean Food and Drug Administration (ranging from 0.5 to 0.6 ppm). Eight real samples collected from the Seoul area were first monitored using SPFIA, and none of them were found positive. These findings are in good accordance with those observed by HPLC analysis. To the best of our knowledge, this is the first report to monitor the aminoglycoside residues in pork meat press juice using SPFIA.

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Section: Methods Validationsupporting

confidence: 86%

Section: Introductionmentioning

confidence: 99%

Monitoring of streptomycin and dihydrostreptomycin residual levels in porcine meat press juice and muscle via solid‐phase fluorescence immunoassay and confirmatory analysis by liquid chromatography after post‐column derivatization

Pyun

El‐Aty

Hashim

et al. 2007

Biomedical Chromatography

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“…Recently, several types of SPE columns have been commonly used for extraction of aminoglycosides in bio-samples, such as a strong-cation exchanger [11,12], a weak-cation exchanger [13,14], an RP C18 [15,16], and a mixed model of an ion exchanger combined with RP [17]. Using SPE column, targeting analytes could be cleaned up, purified, and concentrated easily from a complicated matrix.…”

Section: Introductionmentioning

confidence: 99%

On-line concentration of neomycin and screening aminoglycosides in milk by short capillary column and tandem mass spectrometry

Lu¹,

Feng²

2006

J. Sep. Sci.

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An MS-MS method was established for the trace analysis of neomycin and screening aminoglycoside antibiotics (such as amikacin, gentamicin, kanamycin, and tobramycin) in a milk sample. The extraction and purification are based on ion-pair SPE technology on a short fused-silica capillary RP C18 column. The capillary SPE column provided the stationary phase to retain aminoglycoside antibiotics and MS-MS compatible organic acid heptafluorobutyric acid (HFBA) was used as protein precipitation and ion-pair reagent. Aminoglycosides were extracted in this short column and directly eluted to MS-MS without evaporating to dryness and reconstituted with MS-MS compatible solvent after SPE. The LOQ was 0.1 microg/mL and the calibration curve was linear up to 6.4 microg/mL. A small amount of milk product, 10 microL, is sufficient for the analysis and application of this method as the trace analysis of neomycin in the biological matrix proved simple and workable.

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“…In order to determine withdrawal times with respect to these MRL levels, reliable methods for quantifying DHS in tissues and milk have to be developed and validated. However, the detection of DHS in biological samples, and of aminoglycosides in general, is hampered by its physical and chemical properties: (1) DHS is not volatile, so gas chromatography (GC) is possible only after extensive sample preparation followed by derivatization (acetylation);4–6 (2) DHS lacks any useful chromophores or fluorophores, so detection is usually achieved only after pre‐ or post‐column derivatization when using liquid chromatography (LC), combined with UV or fluorescence detection,7–11 requiring again elaborate sample preparation and lacking sometimes robustness; (3) DHS is too polar to be retained on reversed‐phase (RP) LC stationary phases, unless in combination with ion‐pair chromatography,8–15 implicating a reduced sensitivity when mass spectrometric (MS) detection is used. On the basis of the above, LC‐MS/MS seems to be the method of choice for the detection of such components in biological matrices, since no derivatization is required.…”

Section: Introductionmentioning

confidence: 99%

Quantitative determination of dihydrostreptomycin in bovine tissues and milk by liquid chromatography‐ electrospray ionization‐tandem mass spectrometry

2007

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Dihydrostreptomycin (DHS) is an aminoglycoside antibiotic used in veterinary medicine in combination with benzylpenicillin for the treatment of bacterial infections in cattle, pigs and sheep. A method to determine its residues in edible tissues of cattle, as well as in milk, was developed and validated. Extraction of DHS from the tissues was performed using a liquid extraction with a 10 mM phosphate buffer containing 2% (w/v) trichloroacetic acid, while milk samples were treated with a 50% (w/v) trichloroacetic acid solution, followed by a solid-phase clean-up procedure on a carboxypropyl (CBA) weak cation exchange column. Ion-pair chromatography, using a mixture of 20 mM pentafluoropropionic acid in water and acetonitrile as the mobile phase, was used to retain DHS and the internal standard streptomycin (STR) on a Nucleosil (5 microm) reversed-phase C18 column. The components were detected and quantified by electrospray ionization (ESI) tandem mass spectrometry. The method could be validated according to EC (European Community) requirements with respect to linearity, trueness and precision, the latter evaluated at the maximum residue limit (MRL) - 1000 ng g(-1) for kidney, 500 ng g(-1) for muscle, liver and fat, and 200 ng g(-1) for milk -, at one-half of the MRL and at one and a half times the MRL. A limit of quantification of 10 ng g(-1) and 1 ng ml(-1) was obtained for all tissues and for milk, respectively, which is far below one-half of the MRL as requested, while the limit of detection was in the low ppb range, varying between 1.9 and 4.2 ng g(-1) for the different tissues tested, and being 0.6 ng ml(-1) for milk. The method was used for the monitoring of DHS residues in incurred tissue and milk samples coming from cattle medicated with DHS in combination with benzylpenicillin by intramuscular injection, in order to evaluate withdrawal times.

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Modified determination of dihydrostreptomycin in kidney, muscle and milk by HPLC†

Cited by 24 publications

References 5 publications

Monitoring of streptomycin and dihydrostreptomycin residual levels in porcine meat press juice and muscle via solid‐phase fluorescence immunoassay and confirmatory analysis by liquid chromatography after post‐column derivatization

Monitoring of streptomycin and dihydrostreptomycin residual levels in porcine meat press juice and muscle via solid‐phase fluorescence immunoassay and confirmatory analysis by liquid chromatography after post‐column derivatization

On-line concentration of neomycin and screening aminoglycosides in milk by short capillary column and tandem mass spectrometry

Quantitative determination of dihydrostreptomycin in bovine tissues and milk by liquid chromatography‐ electrospray ionization‐tandem mass spectrometry

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