Synthesis and characterization of oxytetracycline

Authors: Sneha Aggarwal Yudhishthir Singh Rajput Gulab Singh Rajan Sharma

Publish Date: 2015/03/24

Volume: 6, Issue: 2, Pages: 209-214

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Abstract

Magnetic imprinted polymer was prepared by polymerization of methacrylate and ethyleneglycoldimethacrylate in the presence of oxytetracycline on the surface of iron magnetite Selectivity of prepared polymer was calculated from ratio of partition coefficient of oxytetracycline for imprinted and non imprinted polymer in water acetonitrile methanol and at different pH in aqueous buffer pH of solvent exhibited pronounced effect on selectivity Selectivity at pH 70 60 and 50 was 360 225 and 161 fold higher than at pH 40 Imprinted polymer was not selective for oxytetracycline in methanol However selectivity in water and acetonitrile was 1942 and 286 respectively Oxytetracycline did bind to imprinted polymer in water or aqueous buffer pH 70 and could be eluted with methanol Prepared polymer extracted 75–80  oxytetracycline from water honey and egg whiteThe widespread use of antibiotics in dairy cattle poultry and bee keeping leads to presence of antibiotic residues in food chain To prevent any harmful health effects on consumers FAO WHO and European Union have established the maximum residual limits for veterinary drugs Council Regulation 2377/90/EEC Oxytetracycline OTC is a broad spectrum antibiotic against Grampositive and Gramnegative bacteria It is used for the treatment of bacterial brood disease and is the most commonly applied tetracycline group of antibiotics to food producing animals OTC also finds application in human therapy apiculture and fruit crop production Niazi et al 2008 The presence of OTC residue in foods may constitute a variety of public health hazards including toxicological microbiological immunological and pharmacological hazards Navrátilová et al 2009 Frequent use of antibiotic impacts on emergence of antimicrobial resistance creates disorder in intestinal flora and may lead to possible occurrence of allergic reactions HonkanenBuzalski and Reybroeck 1997 Roberts 1997 Cerniglia and Kotarski 2005 Food analysis requires extensive sample preparation prior to its instrumental analysis Ridgway et al 2007 Classical sample preparation technique which involves repeated sample extraction with solvent under shaking followed by centrifugation results in low extraction yield Yan et al 2007 Some high extraction yielding techniques such as pressurized liquid extraction Haglund et al 2007 Soler et al 2007 supercritical fluid extraction JiménezCarmona and Luque de Castro 1998 Rodil et al 2005 microwaveassisted extraction Cheng et al 2007 You et al 2007 and ultrasonicassisted extraction RuizJiménez et al 2004 Rezić et al 2005 have also been applied for food analysis However prepared sample is not suitable for direct instrument analysis and requires one or more prior purification steps Heems et al 1998 Buldini et al 2002 Paleologos and Kontominas 2004 Hamscher et al 2005 Kuhnle et al 2007 Extraction protocol specific to analyte can lead to clean sample preparationMolecular imprinting is a technique which creates stable synthetic polymers possessing tailormade selective recognition sites obtained using high amount of crosslinker in the presence of template molecule Xie et al 2003 Once polymerization is over removal of template from polymer leaves specific cavities which can rebind template selectively on the basis of shape size and functionality Despite the advantages of molecular imprinting polymer such as stability at extreme of pH and temperature ease of preparation low cost and reusability it requires column or prepacked column and negative or positive pressure generating pump or centrifugeThe magnetic polymer is prepared by encapsulating inorganic magnetic particles in organic polymers Yao et al 2008 On integration of magnetic separation technology with imprinted polymer the resulting magnetic polymer will have magnetic properties and selective for template molecule Magnetic separation technology makes separation of analyte easier and faster and also provides large surface to volume ratio The present study reports synthesis and application of OTCimprinted magnetic polymerOTCHCl tetracycline metacycline chlortetracycline cefquinome gentamycin methacrylic acid MAA ethylene glycol dimethacrylate EGDMA oleic acid IronII chloride FeCl2·4H2O Iron III chloride FeCl3·6H2O polyvinylpyrrilidone PVP azobisisobutyronitrile AIBN were purchased from Sigma Aldrich USA Methanol HPLC grade ethanol acetic acid glacial and acetonitrile HPLC grade were procured from Himedia IndiaThe Fe3O4 magnetite was prepared by coprecipitation method as described by Chen and Li 2013 198 g of FeCl2·4H2O and 541 g of FeCl3·6H2O were dissolved in 100 mL of deaerated water The mixture was stirred vigorously and purged with nitrogen gas while temperature was raised to 80 °C Then 40 mL of sodium hydroxide solution 2 N was added dropwise After 1 h magnetic precipitates were separated with help of external magnet and washed several times with deaerated water After washing precipitates were dried at 60 °C 1 g Fe3O4 magnetite freshly prepared and 10 mL oleic acid were mixed Then 377 mL EGDMA was added and mixed

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