Identification of medicinal additives in animal feedingstuffs by high-performance liquid chromatography

Cody, Maria K.; Clark, Georgina B.; Conway, Brian; Crosby, Neil

doi:10.1039/an9901500001

Cited by 10 publications

(3 citation statements)

References 3 publications

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“…Improved recovery of antimicrobials from animal feedingstu s by the addition of a small amount of aqueous phase (5%) to the extraction solvent prior to determination by HPLC has been reported by Cody et al (1990) who suggested that the presence of the small amount of water allowed better penetration of the sample matrix by the extractant. The relatively aqueous nature of the extractant used in the IST should result in good matrix penetration suggesting that the failure to detect some compounds is more likely to be due to their poor solubility in the extractant rather than poor matrix penetration.…”

Section: Discussionmentioning

confidence: 95%

Evaluation of a single plate microbiological growth inhibition assay as a screening test for the presence of antimicrobial agents in compound animal feedingstuffs at therapeutic and contaminating concentrations

Higgins

McEvoy²,

Lynas³

et al. 1999

Food Additives and Contaminants

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The Inhibitory Substance Test (IST), a microbiological growth inhibition test, is used for screening animal feedingstuffs for the presence of (contaminating) antimicrobial compounds. The effectiveness of the IST was established for 33 compounds that may be incorporated in feedingstuffs. Minimum detectable concentrations (MDCs) for standard solutions were established and compared with those obtained following solvent extraction of an antimicrobial-free compound feedingstuff spiked with each compound at 0-20 mg/kg. Of the 33 standard solutions examined, the test organism was not sensitive to 11 and the MDC for one was greater than its maximum inclusion rate in complete feedingstuffs. Following routine extraction (25% acetone-phosphate buffer) of feedingstuffs spiked with each of the 22 compounds to which the organism was sensitive, 10 were not detected, 15 were detectable at both minimum and maximum feed-inclusion rates and four were only detectable at their maximum feed-inclusion rates. Extraction with methanol (25%) had a deleterious effect with 12 compounds not detected, nine detectable at both minimum and maximum feed-inclusion rates and five detectable at their maximum feed-inclusion rates. Increasing acetone and methanol concentrations to 40 and 55% respectively resulted in larger inhibitory zones for antibiotic-free feedingstuff (25.3 + 2.43 mm vs 21.1 + 1.02 mm) compared with both 25% acetone (11.3 + 0.22 mm) and 25% methanol (11.2 + 0.22 mm), requiring the establishment of greater threshold zone diameters and negating any advantage in increasing the solvent concentration under these test conditions. It is concluded that the IST may be particularly useful for detection of a number of the zootechnical feed-additives recently banned in the EU, which, if used illegally, may be present at sufficiently high inclusion rates to facilitate detection. Further alteration of extraction conditions may improve the scope of the assay.

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Section: Discussionmentioning

confidence: 95%

Evaluation of a single plate microbiological growth inhibition assay as a screening test for the presence of antimicrobial agents in compound animal feedingstuffs at therapeutic and contaminating concentrations

Higgins

McEvoy²,

Lynas³

et al. 1999

Food Additives and Contaminants

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“…In animal production, nifursol was illegally added in feed for feeding animals. All of the reported methods to detect nifursol (parent drug) were high-performance liquid chromatography (HPLC) methods (Cody, Clark, Conway, & Crosby, 1990;De Vries, Cas, & Kuil, 1994). Though the stability of chromatographic analysis is good, the sample preparation procedure is complicated and skilled operators are needed.…”

Section: Introductionmentioning

confidence: 99%

Monoclonal antibody-based fluorescence polarisation immunoassay for nifursol in feed

Zhang¹,

Shen²,

Zhong³

2010

Food and Agricultural Immunology

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Novel tracers were designed and then used to develop a rapid, specific and sensitive fluorescence polarisation immunoassay (FPIA) method to detect nifursol in feed. The 3-((2-(2-hydroxy-3,5-dinitrobenzoyl)hydrazono)methyl)benzoic acid was used for the production of immunogen and 3,5-dinitrosalicylic acid was used for synthesis of fluorescein-labelled tracer. Based on monoclonal antibody and tracer, an optimised FPIA method was established with IC 50 of 5.0 ng mL (1 , and low cross-reactivity with other nitrofurans ( B0.05%). FPIA provides a suitable means for screening of a large number of samples. The limits of detection calculated from the analysis of 20 known negative feed samples (pig feed, chicken feed and fish feed) were 0.4Á0.8 ng g (1 (mean'3 SD). Recoveries of nifursol fortified ranged from 85.0 to 95.0%. The coefficients of variation were less than 10%.

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“…To date, chromatographic methods to detect dinitolmide and 3‐ANOT residues rely primarily on high‐performance liquid chromatography (HPLC), ultra‐performance liquid chromatography, and liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) . However, there are few reports describing the chromatographic detection of dinitolmide residues in eggs, and most analytical methods are only designed to detect the prototype drug.…”

Section: Introductionmentioning

confidence: 99%

Development of an ASE‐GC‐MS/MS method for detecting dinitolmide and its metabolite 3‐ANOT in eggs

et al. 2018

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An accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry (ASE-GC-MS/MS) method for detecting dinitolmide residue and its metabolite (3-amino-2-methyl-5-nitrobenzamide, 3-ANOT) in eggs was developed and optimized. The samples were extracted using ASE with acetonitrile as the extractant and were purified by passage through a neutral alumina solid-phase extraction column. Then, the samples were analyzed using the GC-MS/MS method. The optimized method parameters were validated according to the requirements set forth by the European Union and the Food and Drug Administration. The average recoveries of dinitolmide and 3-ANOT from eggs (egg white, egg yolk, and whole egg) at the limit of quantification (LOQ), 0.5 maximum residue limit (MRL), 1 MRL, and 2 MRL were 82.74% to 87.49%, the relative standard deviations (RSDs) were less than 4.63%, and the intra-day RSDs and the inter-day RSDs were 2.96% to 5.21% and 3.94% to 6.34%, respectively. The limits of detection and the LOQ were 0.8 to 2.8 μg/kg and 3.0 to 10.0 μg/kg, respectively. The decision limits (CC ) were 3001.69 to 3006.48 μg/kg, and the detection capabilities (CC ) were 3001.74 to 3005.22 μg/kg. Finally, the new method was successfully applied to the quantitative determination of dinitolmide and 3-ANOT in 50 commercial eggs from local supermarkets.

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Identification of medicinal additives in animal feedingstuffs by high-performance liquid chromatography

Cited by 10 publications

References 3 publications

Evaluation of a single plate microbiological growth inhibition assay as a screening test for the presence of antimicrobial agents in compound animal feedingstuffs at therapeutic and contaminating concentrations

Evaluation of a single plate microbiological growth inhibition assay as a screening test for the presence of antimicrobial agents in compound animal feedingstuffs at therapeutic and contaminating concentrations

Monoclonal antibody-based fluorescence polarisation immunoassay for nifursol in feed

Development of an ASE‐GC‐MS/MS method for detecting dinitolmide and its metabolite 3‐ANOT in eggs

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