Marunaka T, Shibata T, Minami Y, Umeno Y
J Chromatogr. 1980 Sep 12;183(3):331-8. doi: 10.1016/s0378-4347(00)81713-2.
A high-performance liquid chromatographic method was developed for the simultaneous determination of phenylbutazone and its metabolites, oxyphenbutazone and gamma-hydroxy-phenylbutazone, in plasma and urine. Samples were acidified with hydrochloric acid and extracted with benzene--cyclohexane (1:1, v/v). The extract was redissolved in methanol and chromatographed on a muBondapak C18 column using a mobile phase of methanol--0.01 M sodium acetate buffer (pH 4.0) in a linear gradient (50 to 100% methanol at 5% min; flow-rate 2.0 ml/min) in a high-performance liquid chromatograph equipped with an ultraviolet absorbance detector (254 nm). The detection limit for phenylbutazone, oxyphenbutazone and for gamma-hydroxyphenylbutazone was 0.05 microgram/ml. A precise and sensitive assay for the determination of phenylbutazone and its metabolites was established.
建立了一种高效液相色谱法,用于同时测定血浆和尿液中的保泰松及其代谢物羟基保泰松和γ-羟基保泰松。样品用盐酸酸化,并用苯 - 环己烷(1:1,v/v)萃取。萃取物重新溶解于甲醇中,并在配备紫外吸收检测器(254nm)的高效液相色谱仪上,使用甲醇 - 0.01M醋酸钠缓冲液(pH 4.0)的流动相,以线性梯度(5%分钟内从50%到100%甲醇;流速2.0ml/min)在μBondapak C18柱上进行色谱分析。保泰松、羟基保泰松和γ-羟基保泰松的检测限为0.05微克/毫升。建立了一种用于测定保泰松及其代谢物的精确且灵敏的分析方法。