首页> 中文期刊>分析测试学报 >高效液相色谱-二极管阵列检测法同时分析兽药粉剂中11种磺胺类药物

高效液相色谱-二极管阵列检测法同时分析兽药粉剂中11种磺胺类药物

     

摘要

A novel method was developed for the simultaneous determination of 11 sulfonamides in veterinary pharmaceutical powder by high performance liquid chromatography - diode array detection. The sample was extracted with 95% acetonitrile solution and then purified by an Alumina - B solid phase extraction cartridge. The extraction residue was redissolved in 15% acetonitrile solution and separated on a TC - C18 chromatographic column. The mobile phase was composed of 0.017 mol/L phosphoric acid and acetonitrile and a gradient elution program was carried out. The diode assay detection was used for the qualitative and quantitative analysis. The results indicated that the chromatographic peaks of 11 sulfonamides drugs and their corresponding spectra were ideal under the optimal conditions. The calibration curves of 11 ana-lyte were linear in the range of 0.25 -10.0 mg/L. The average recoveries of 11 sulfonamides at three spiked levels of 0.5, 1.0, 5.0 mg/kg were between 67% and 97% , with relative standard deviations ranged from 1.5% to 9.9% . Based on signal to noise ratio(S/N =3) and the corresponding spectra, the limits of detection of 11 analytes in veterinary pharmaceutical powder were all 0. 25 mg/kg.%建立了高效液相色谱-二极管阵列检测法同时测定兽药粉剂中11种磺胺类药物的分析方法.试样采用95%乙腈提取,经碱性氧化铝固相萃取小柱净化,15%乙腈复溶残渣后用Agilent TC - C18色谱柱分离,0.017 mol/L磷酸溶液和乙腈为流动相进行梯度洗脱,二极管阵列检测器进行检测.结果表明,在优化实验条件下,11种磺胺类药物的色谱分离和相应光谱图匹配理想;在0.25~ 10.0 mg/L范围内线性关系良好;兽药粉剂中添加0.5~ 5.0 mg/kg水平的11种磺胺类药物的回收率在67%~ 97%之间,相对标准偏差为1.5%~9.9%;以3倍信噪比(S/N=3)结合相应光谱图计算得11种磺胺类药物的检出限均为0.25 mg/kg.

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