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Direct determination of ampicillin and amoxicillin residues in food samples after aqueous SDS extraction by micellar liquid chromatography with UV detection

机译:胶束液相色谱-紫外检测法直接测定水样SDS萃取后食品中氨苄西林和阿莫西林残留量的直接测定

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A simple, sensitive and rapid micellar HPLC method was optimized and validated for the analysis of amoxicillin and ampicillin residues in food samples. Analytical separation was performed in less than 7 min using a RP C18 column with UV detection at 220 nm and a micellar solution of 0.05 M sodium dodecyl sulphate, 5% 1-propanol and 0.3% triethylamine in 0.02 M phosphoric acid buffered at pH 5 as the mobile phase. The flow rate was 1 mL mina?’1 and the effluent was monitored at 220 nm. The micellar method was successfully applied to quantitatively determine amoxicillin and ampicillin residues in spiked chicken muscles, chicken liver, bovine muscles, liver, kidney and eggs. The method was fully validated in accordance with ICH guidelines. Linearity was in the range 0.4a€“20 ??g mLa?’1 for each drug and the percentage recoveries of both drugs ranged from 95.5 to 102.3% for amoxicillin and 95.6 to 101.7% for ampicillin. High extraction efficiency of amoxicillin and ampicillin was obtained without matrix interference in the extraction process and in the subsequent chromatographic determination. An aqueous solution of SDS surfactant only was used in extraction. No organic solvent was used during the pretreatment step. Hence, it is considered an interesting technique for a€?greena€? chemistry.
机译:优化并验证了一种简单,灵敏,快速的胶束HPLC方法,用于分析食品样品中的阿莫西林和氨苄青霉素残留。使用RP C18色谱柱在不到7分钟的时间内进行分析分离,该色谱柱在220 nm处有UV检测,并用0.05 M的十二烷基硫酸钠,5%的1-丙醇和0.3%的三乙胺的胶束溶液溶于pH值为5的0.02 M磷酸中。流动相。流速为1 mL min-1 ?,并在220 nm处监测流出液。胶束法已成功用于定量测定加标的鸡肌肉,鸡肝,牛肌肉,肝,肾和卵中的阿莫西林和氨苄青霉素残留。该方法已按照ICH指南进行了充分验证。每种药物的线性均在0.4a€“ 20?g mLa?'1的范围内,两种药物的回收百分率对阿莫西林为95.5至102.3%,对氨苄西林为95.6至101.7%。获得了阿莫西林和氨苄青霉素的高提取效率,在提取过程和随后的色谱测定中没有基质干扰。仅将SDS表面活性剂的水溶液用于提取。在预处理步骤中不使用有机溶剂。因此,它被认为是“绿色”的有趣技术。化学。

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