Horie M, Saito K, Hoshino Y, Nose N, Hamada N, Nakazawa H
Saitama Prefectural Institute of Public Health, Japan.
J Chromatogr. 1990 Mar 2;502(2):371-8. doi: 10.1016/s0021-9673(01)89601-1.
A simple and selective method for the determination of sulphamethazine (SMT) and its metabolite, N4-acetylsulphamethazine (N4-AcSMT), in meat by high-performance liquid chromatography (HPLC) with photodiode-array detection was developed. The drugs were extracted from meat with 0.2% metaphosphoric acid-methanol (6:4), followed by a Bond-Elut C18 clean-up procedure. The HPLC separation was carried out on a Supersphere RP-18e column (125 X 4.0 mm I.D.) using 0.05 M sodium dihydrogenphosphate (pH 4.5)-acetonitrile (8:2) as the mobile phase at a flow-rate of 0.5 ml/min, and monitored with a photodiode-array detector. The recoveries of SMT and N4-AcSMT from meat fortified at 0.5 micrograms/g were 90.1-93.3 and 93.0-94.4%, respectively, with coefficients of variation of 1.9-3.2 and 1.5-2.7%. The limits of detection were 0.02 micrograms/g for each drug. SMT was found in ten samples of imported meat (12.5%) at levels ranging from 0.05 to 1.05 micrograms/g.
建立了一种简单且具选择性的方法，用于通过带光电二极管阵列检测的高效液相色谱法（HPLC）测定肉类中的磺胺二甲嘧啶（SMT）及其代谢物N4-乙酰磺胺二甲嘧啶（N4-AcSMT）。用0.2%偏磷酸-甲醇（6:4）从肉类中提取药物，随后进行Bond-Elut C18净化程序。HPLC分离在Supersphere RP-18e柱（125×4.0 mm内径）上进行，使用0.05 M磷酸二氢钠（pH 4.5）-乙腈（8:2）作为流动相，流速为0.5 ml/min，并采用光电二极管阵列检测器进行监测。在添加量为0.5微克/克的强化肉类中，SMT和N4-AcSMT的回收率分别为90.1 - 93.3%和93.0 - 94.4%，变异系数分别为1.9 - 3.2%和1.5 - 2.7%。每种药物的检测限为0.02微克/克。在十个进口肉类样品（占12.5%）中发现了SMT，含量范围为0.05至1.05微克/克。
