HPLC-PDA法同时测定硫酸新霉素可溶性粉中非法添加4种化学药物
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摘要
建立了同时测定硫酸新霉素可溶性粉中非法添加甲硝唑、水杨酸、乙酰甲喹、甲氧苄啶的HPLC-PDA方法。样品用甲醇提取,经C18柱分离,以磷酸盐缓冲液-甲醇为流动相洗脱,流速为1.0 m L/min,采用二极管阵列检测器进行全波长(200~400 nm)扫描,提取波长为230 nm。检查保留时间、峰纯度和光谱相似度,对非法添加化学药物进行确证。结果表明,4种化学药物在0.01~0.12 mg/m L范围内线性关系良好(r≥0.9998);回收率在98.0%~99.9%之间,RSD≤1.0%,检出限为1~5 g/kg。该检测方法专属性强、操作简便,可用于硫酸新霉素可溶性粉中非法添加4种化学药物的测定。
To establish a method for simultaneous determination of illegally adding metronidazole,salicylic acid,mequindox and trimethoprim in neomycin sulfate soluble powder by the high performance liquid chromatography with photo-diode array detector( HPLC-PDA),samples were extracted by methanol. C18 column was applied with mobile phase consisting of sodium dihydrogen phosphate buffer-methanol( 70 ∶ 30) at a flow rate of 1.0 m L/min.The extract wavelength was 230 nm from the scanning of 200 ~ 400 nm by photo-diode array detector. Retention time,peak purity test and spectral similarity were helped to identify the four kinds of target analytes. The linearity in the correlation range of 0. 01 ~ 0. 12 mg/m L were good( r ≥0. 9998). The recoveries ranged from 98. 0% to99.9% with the relative stand deviations( RSDs) all below 1.0%. The limits of detection were from 1 to 5 g/kg. In conclusion,the method has good specifity and simple treatment,and can be used as a reliable way for detecting drugs adulterated in neomycin sulfate soluble powder.
To establish a method for simultaneous determination of illegally adding metronidazole,salicylic acid,mequindox and trimethoprim in neomycin sulfate soluble powder by the high performance liquid chromatography with photo-diode array detector( HPLC-PDA),samples were extracted by methanol. C18 column was applied with mobile phase consisting of sodium dihydrogen phosphate buffer-methanol( 70 ∶ 30) at a flow rate of 1.0 m L/min.The extract wavelength was 230 nm from the scanning of 200 ~ 400 nm by photo-diode array detector. Retention time,peak purity test and spectral similarity were helped to identify the four kinds of target analytes. The linearity in the correlation range of 0. 01 ~ 0. 12 mg/m L were good( r ≥0. 9998). The recoveries ranged from 98. 0% to99.9% with the relative stand deviations( RSDs) all below 1.0%. The limits of detection were from 1 to 5 g/kg. In conclusion,the method has good specifity and simple treatment,and can be used as a reliable way for detecting drugs adulterated in neomycin sulfate soluble powder.
引文
[1]中国兽药典委员会.中华人民共和国兽药典2015年版(一部)[S].Commission of Chinese Veterinary Pharmacopoeia. Veterinary Pharmacopoeia of the People's Republic of China(the first volume of 2015 edition)[S].
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[2]中国兽药典委员会.兽药质量标准(2017年版)化学药品卷[S].Commission of Chinese Veterinary Pharmacopoeia.Quality Standard for Veterinary Drugs,2017,Chemical Medicine Volume[S].
[3]中国兽药典委员会.中华人民共和国兽药典兽药使用指南化学药品卷2010年版[S].Commission of Chinese Veterinary Pharmacopoeia Guide to Utilization of Veterinary Drug in Veterinary Pharmacopoeia of Pecple's Republic of China,2017,Chemical Medicine Volume[S].
[4]国家农业部官网.农业部持续创新兽药抽检制度加快提升兽药产品质量水平[EB/OL]. http://www.moa.gov.cn/xw/zwdt/201503/t20150316_4440988.htm.Official Website of Ministry of Agriculture. The Ministry of Agriculture continues to innovate the sampling system of veterinary drugs to accelerate the improvement of veterinary drug product quality level[EB/OL]. http://www. moa. gov. cn/xw/zwdt/201503/t20150316_4440988.htm.
[5]农医发[2017]2号文农业部关于印发《2017年兽药质量监督抽检计划》的通知[Z].Agricultural medicine[2017]2 paper on the ministry of Agriculture issued 2017 quality supervision and sampling of veterinary drugs plan notice[Z].
[6]戴青,于丽娜,张璐,等.硫酸安普霉素可溶性粉中非法添加乙酰甲喹的HPLC-PDA检测方法的建立[J].中国兽药杂志,2017,51(2):19-23.Dai Q,Yu L N,Zhang L,et al. Dtermination of Mequindox in Apramycin Sulfate Soluble Power by HPLC-PDA[J]. Chinese Journal of Veternary,2017,51(2):19-23.
[7]农业部.中华人民共和国农业部公告2448号[S].Minstery of Agriculture. No. 2448. Bullerion of the Minstery of Agriculture of the People's Republic[S].