Sample preparation strategy for the simultaneous determination of macrolide antibiotics in animal feedingstuffs by liquid chromatography with electrochemical detection (HPLC-ECD)

Huebra, Marı́a José González de la; Vincent, Ursula; Holst, Christoph von

doi:10.1016/j.jpba.2006.12.008

Cited by 44 publications

(24 citation statements)

References 21 publications

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“…Lower LOD values for these drugs in animal feedingstuffs were also observed by De la Huebra et al [15] . The CCα (130.6 µg kg -1 ) and CCβ (136.2 µg kg -1 ) values for tylosin obtained in animal feedingsuffs were better than those reported by Van Poucke et al [16] .…”

Section: Discussionsupporting

confidence: 72%

“…These values could be considered satisfactory, on account of the complexity of the biological matrices. Higher-than-average recoveries for ERY, SPI, TIL and TYL [15] ; for ERY and TYL [17] have also been reported for animal feedingstuffs. However, lower-than-average recoveries for TIL in pig feed samples were also observed by Kaklamanos et al [18] .…”

Section: Discussionmentioning

confidence: 99%

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Determination of Erythromycin, Spiramycin, Tilmicosin and Tylosin in Animal Feedingstuffs by Liquid Chromatography-Tandem Mass Spectrometry

Yibar¹,

Özcan²,

Karaca³

2014

Kafkas Univ Vet Fak Derg

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Detection of macrolides residues in animal feedingstuffs to ensure food safety is very important issue. For this purpose, a liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of residues of 4 macrolides (erythromycin, spiramycin, tilmicosin and tylosin) in animal feedingstuffs. Roxithromycin (ROX), a macrolide not used in veterinary medicine, was used as internal standard. The mass spectral acquisition was done in the positive-ion mode applying multiple reaction monitoring with the following ions (mass-to-charge ratio, m/z): m/z 837.4→679.2; m/z 734.4→576.2; m/z 422.4→174.1; m/z 869.1→696.1 and m/z 916.4→772.4 for roxithromycin (ROX), erythromycin (ERY), spiramycin (SPI), tilmicosin (TIL), and tylosin (TYL), respectively. Good repeatibility, reproducibility and recovery values was obtained. Average recoveries ranged from 98.9% (TIL) to 101% (ERY) and an overall mean of 99.9%. Method limits of detection (LODs) of ERY, SPI, TIL and TYL 5.1, 6.6, 6.7 and 7.5 µg kg-1 were achieved respectively. Method limits of quantification (LOQs) were 8.5, 11.1, 11.2 and 12.4 µg kg-1 for the same drugs, respectively. Satisfactory decision limits (CCα) and detection capabilities (CCβ) were also attained. The method is simple, rapid, sensitive and suitable for the simultaneous determination of macrolide antibiotics in animal feedingstuffs. Keywords: Macrolides, Feedingstuffs, Validation, LC-MS/MS Hayvan Yemlerinde Eritromisin, Spiramisin, Tilmikosin ve Tilosinin LC-MS/MS İle Tespiti ÖzetMakrolid grubu antibiyotiklerin hayvan yemlerinde tespit edilmesi gıda güvenliğinin sağlanması açısından çok önemli bir konudur. Bu amaçla, hayvan yemlerinde kullanılan 4 adet makrolid (eritromisin, spiramisin, tilmikosin ve tilosin)'in tespiti için sıvı kromatografi-tandem kütle spektrometrisi (LC-MS/MS) metodu valide edilerek kullanılmıştır. Roksitromisin (ROX), veteriner hekimlik alanında kullanılmayan bir makroliddir ve bu yüzden çalışmada iç standart olarak kullanılmıştır. Kütle spektrası uygulaması pozitif-iyon modunda ve çoklu reaksiyon izleme modunda gerçekleştirilerek, (kütle/şarj oranı, m/z) roksitromisin (ROX) için m/z 837.4→679.2; eritromisin (ERY) için m/z 734.4→576.2; spiramisin (SPI) için m/z 422.4→174.1; tilmikosin (TIL) için m/z 869.1→696.1 ve tilosin (TYL) için m/z 916.4→772.4 taranmıştır. İyi bir tekrarlanabilirlik, üretilebilirlik ve geri kazanım değerleri elde edildi. Hesaplanan ortalama geri kazanım değerleri %98.9 (TIL)'den %101'e (ERY) kadar değişmekle beraber, toplam ortalama %99.9 olarak gerçekleşti. Metodun tespit limitleri (LOD) ERY, SPI, TIL ve TYL için sırasıyla, 5.1, 6.6, 6.7 and 7.5 µg kg-1 olarak hesaplandı. Metodun sayı verilebilir limitleri aynı sırayla 8.5, 11.1, 11.2 and 12.4 µg kg-1 olarak gerçekleşti. Validasyon sonucunda belirtilen bu dört makrolid için memnun edici karar limitleri (CCα) ve karar verebilme kapasitelerine (CCβ) de ulaşılabildi. Validasyon sonuçlarına bakıldığında basit, hızlı, duyarlı ve uygun olan bu metot yukarıda belirtilen dört...

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Section: Discussionsupporting

confidence: 72%

Section: Discussionmentioning

confidence: 99%

Determination of Erythromycin, Spiramycin, Tilmicosin and Tylosin in Animal Feedingstuffs by Liquid Chromatography-Tandem Mass Spectrometry

Yibar¹,

Özcan²,

Karaca³

2014

Kafkas Univ Vet Fak Derg

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“…Beside those methods there is still a practical interest in developing alternative methods, the socalled postscreening methods, aimed to further reduce the number of samples submitted to confirmatory analysis. These methods have performance characteristics between the requirements of the screening and the confirmatory methods [17,29,48].…”

Section: Analytical Strategiesmentioning

confidence: 99%

“…The cartridge was washed with phosphate buffer solution, CAP was eluted with 20% v/v MeOH in ethyl acetate and the first 0.5 mL of the eluate was discarded. [48].…”

Section: Analytical Strategiesmentioning

confidence: 99%

Chromatographic analysis of banned antibacterial growth promoters in animal feed

Samanidou¹,

Evaggelopoulou

2008

J of Separation Science

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The issue of antimicrobial use in animals used as food is of global concern. Antimicrobials are used in animal agriculture to improve health and welfare of animals, meat quality, the economic efficiency of growth and production and public health by decreasing shedding of zoonotic pathogens. However, large quantities are often used without professional supervision. The growth-promotant (now reclassified as zootechnical feed additives) effect of low levels of antibiotics in animal feeds was first described in the late 1940s. Already in 1969 the Swann Committee recommended that use of antibiotics as a supplement in animal feedstuff should be restricted to those with little or no application as therapeutic agents for humans and animals, which would not impair the efficacy of therapeutic antibiotics through the development of resistant strains of organisms. Antimicrobials like avoparcin, ardacin, zinc bacitracin, virginiamycin, tylosin, spriramycin, carbadox and olaquindox were withdrawn within the period 1997-1999. Four others (monensin sodium, salinomycin sodium, avilamycin and flavophospholipol) were still permitted for use as growth promoters in animal feed to animals marketed in the European Union (EU). Since January 2006, they have been banned as well. This review focuses on the analytical methods developed to be an effective tool for monitoring compliance with the ban.

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“…These methods were time-consuming, tedious, and dedicated to sophisticated and expensive analytical instruments. Many LC methods have been applied to multiresidue analysis of macrolides in biological samples (Gonzalez de la Huebra et al, 2007;Dubois et al, 2001), and no reversed-phase LC methods have been reported for the simultaneous determination of the three macrolides in routine pharmaceutical dosage forms.…”

Section: Introductionmentioning

confidence: 99%

Quantification of three macrolide antibiotics in pharmaceutical lots by HPLC: Development, validation and application to a simultaneous separation

Mahmoudi

Francia

Boukhechem

et al. 2016

British Journal of Pharmacy

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ARTICLE INFO ABSTRACTA new validated high performance liquid chromatographic (HPLC) method with rapid analysis time and high efficiency, for the analysis of erythromycin, azithromycin and spiramycin, under isocratic conditions with ODB RP18 as a stationary phase is described. Using an eluent composed of acetonitrile -2-methyl-2-propanol -hydrogenphosphate buffer, pH 6.5, with 1.5% triethylamine (33:7: up to 100, v/v/v), delivered at a flow-rate of 1.0 mL min -1 . Ultra Violet (UV) detection is performed at 210 nm. The selectivity is satisfactory enough and no problematic interfering peaks are observed. The procedure is quantitatively characterized and repeatability, linearity, detection and quantification limits are very satisfactory.The method is applied successfully for the assay of the studied drugs in pharmaceutical dosage forms as tablets and powder for oral suspension. Recovery experiments revealed recovery of 97.13-100.28%.

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Sample preparation strategy for the simultaneous determination of macrolide antibiotics in animal feedingstuffs by liquid chromatography with electrochemical detection (HPLC-ECD)

Cited by 44 publications

References 21 publications

Determination of Erythromycin, Spiramycin, Tilmicosin and Tylosin in Animal Feedingstuffs by Liquid Chromatography-Tandem Mass Spectrometry

Determination of Erythromycin, Spiramycin, Tilmicosin and Tylosin in Animal Feedingstuffs by Liquid Chromatography-Tandem Mass Spectrometry

Chromatographic analysis of banned antibacterial growth promoters in animal feed

Quantification of three macrolide antibiotics in pharmaceutical lots by HPLC: Development, validation and application to a simultaneous separation

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