Yu Hu, Mu Hui, Hu Ying-Mei
Chemistry Department of Science School, Xi'an Jiaotong University, Xi'an 710049, China.
J Pharm Anal. 2012 Feb;2(1):76-81. doi: 10.1016/j.jpha.2011.09.007. Epub 2011 Nov 4.
An efficient method is provided to detect simultaneously some important veterinary drugs from different classes in highly complex animal tissue matrix. This method using matrix solid-phase dispersion (MSPD) and high performance liquid chromatography (HPLC) with diode array detection (DAD) is developed to effectively determine two fluoroquinolones (enoxacin and lomefloxacin), two sulfonamides (sulfanilamide and sulfamethoxazole) and one tetracycline (tetracycline) simultaneously in porcine tissues. In the process, MSPD methodology was used to treat samples, washed by -hexane to remove lipid, eluted the analytes with acetonitrile-dichloromethane (1:1, v/v). Solvent acetonitrile and solvent acetic acid (0.1%) were combined in a gradient. HPLC-DAD analysis of the tissue samples was performed within 15 min at a flow rate of 1.0 mL/min. The results showed that a recovery at 0.1, 0.5 and 1.0 μg/g fortification levels ranged from 80.6% to 99.2% with satisfactory relative standard deviations (RSDs) (below 6.1%, =3) and the limits of quantitation (LOQ) ranged from 7 μg/kg to 34 μg/kg in porcine tissues. Utilization of the method in successfully simultaneous analysis of porcine tissue incurred with veterinary drug multiresidues is described.
提供了一种高效方法,可在高度复杂的动物组织基质中同时检测不同类别的一些重要兽药。该方法采用基质固相分散(MSPD)和配有二极管阵列检测(DAD)的高效液相色谱(HPLC),用于有效同时测定猪组织中的两种氟喹诺酮类药物(依诺沙星和洛美沙星)、两种磺胺类药物(磺胺和磺胺甲恶唑)以及一种四环素类药物(四环素)。在此过程中,采用MSPD方法处理样品,用正己烷洗涤以去除脂质,用乙腈 - 二氯甲烷(1:1,v/v)洗脱分析物。溶剂乙腈和溶剂乙酸(0.1%)按梯度混合。以1.0 mL/min的流速在15分钟内对组织样品进行HPLC - DAD分析。结果表明,在0.1、0.5和1.0 μg/g的加标水平下,回收率在80.6%至99.2%之间,相对标准偏差(RSD)令人满意(低于6.1%,n = 3),猪组织中的定量限(LOQ)在7 μg/kg至34 μg/kg之间。描述了该方法在成功同时分析含有兽药多残留的猪组织中的应用。