Spahn-Langguth H, Hahn G, Mutschler E
Pharmakologisches Institut für Naturwissenschaftler, Johann Wolfgang Goethe-Universität, Frankfurt/M.
Arch Pharm (Weinheim). 1991 Jul;324(7):445-7. doi: 10.1002/ardp.19913240708.
Piretanide was determined from plasma and urine using reversed-phase high-performance liquid chromatography. Plasma was extracted with diethylether at pH 4 using bumetanide as internal standard. The chromatographic separation was performed on an octadecylsilane column (ODS) with acetonitrile/pH 7 phosphate buffer (3:7, v/v). In order to determine piretanide in urine, bumetanide was added to a urine aliquot. Then the sample was centrifuged and the supernatant directly injected without extraction followed by chromatography on an ODS column with a mixture of methanol and pH 7 phosphate buffer (12:13, v/v). The compounds were detected by their intrinsic fluorescence, monitoring the eluate at 287/450 nm. Total chromatography times were 8 min for plasma and 13 min for urine samples. The method was applied for the assay of piretanide in plasma of healthy volunteers after i.v. or p.o. dosage of 6 mg piretanide.
使用反相高效液相色谱法从血浆和尿液中测定吡咯他尼。以布美他尼为内标,在pH 4条件下用二乙醚萃取血浆。在十八烷基硅烷柱(ODS)上,以乙腈/pH 7磷酸盐缓冲液(3:7,v/v)进行色谱分离。为了测定尿液中的吡咯他尼,向一份尿液中加入布美他尼。然后将样品离心,上清液不经萃取直接进样,随后在ODS柱上用甲醇和pH 7磷酸盐缓冲液(12:13,v/v)的混合物进行色谱分析。通过其固有荧光检测化合物,在287/450 nm处监测洗脱液。血浆的总色谱时间为8分钟,尿液样品为13分钟。该方法用于静脉注射或口服6毫克吡咯他尼后健康志愿者血浆中吡咯他尼的测定。