Furusawa N
Faculty of Human Life Science, Osaka City University, Japan.
J Chromatogr A. 2000 Nov 17;898(2):185-91. doi: 10.1016/s0021-9673(00)00843-8.
A simplified determining/identifying method for residual sulphamethazine (SMZ) and sulphadimethoxine (SDM) in milk by using a high-performance liquid chromatography (HPLC) with a photo-diode array detector was presented. Both sulphonamides in cow's milk samples were extracted by only stirring with ethanol followed by an Ultrafree-MC/Biomax as a centrifugal ultra-filtration unit. For determination/identification of SMZ and SDM, a Mightysil RP-18 GP Aqua column and a mobile phase of 25% (v/v) ethanol solution (in water) with a photo-diode array detector was used. Average recoveries from spiked SMZ and SDM (10-1000 ng/ml each drug) were > or = 83% with the relative standard deviations between 1.4 and 3.7%. The limit of quantitation (LOQ) were calculated to be 5 ng/ml for SMZ and 10 ng/ml for SDM, respectively. The values were below the MRL/tolerance (SMZ, 25 ng/ml; SDM, 10 ng/ml). The total time and solvent required for the analysis of one sample were <35 min and <2 ml of only ethanol, respectively. No toxic solvents were used. The developed procedure was harmless to the human and environment.
提出了一种使用配备光电二极管阵列检测器的高效液相色谱法（HPLC）测定/鉴定牛奶中残留磺胺二甲嘧啶（SMZ）和磺胺二甲氧嘧啶（SDM）的简化方法。牛奶样品中的两种磺胺类药物仅通过与乙醇搅拌提取，然后使用Ultrafree-MC/Biomax作为离心超滤装置。为了测定/鉴定SMZ和SDM，使用了Mightysil RP-18 GP Aqua柱和25%（v/v）乙醇溶液（溶于水）的流动相以及光电二极管阵列检测器。加标SMZ和SDM（每种药物浓度为10 - 1000 ng/ml）的平均回收率≥83%，相对标准偏差在1.4%至3.7%之间。计算得出SMZ的定量限（LOQ）为5 ng/ml，SDM为10 ng/ml。这些值低于最大残留限量/耐受量（SMZ为25 ng/ml；SDM为10 ng/ml）。分析一个样品所需的总时间和溶剂分别小于35分钟和小于2 ml乙醇。未使用有毒溶剂。所开发的方法对人和环境无害。
