Hasegawa H, Takahara E, Yamada T, Nagata O
Research and Development Division, Hokariku Seivaku Co. Ltd., Fukui, Japan.
J Chromatogr B Biomed Appl. 1996 Dec 13;687(2):419-25. doi: 10.1016/s0378-4347(96)00251-4.
A simple and sensitive method for quantitation of HSR-609 (I) in human plasma and urine was developed using HPLC with the fluorescence labelling reagent 4-(N,N-dimethylaminosulfonyl)-7-N-piperazino-2,1,3-benzox adi azole (DBD-PZ). Compound I was extracted from human plasma and urine, and derivatized by reaction with DBD-PZ in the presence of Mukaiyama reagent A, an equimolar solution of 2,2'-dipyridyl disulfide (DPDS) and triphenylphosphine (TPP) in acetonitrile. The reaction mixture was cleaned up by liquid liquid extraction following the derivatization. The conjugate was analyzed by ion-pair-HPLC with fluorometric detection. The quantitation limits for I were 0.5 ng/ml in plasma and 5 ng/ml in urine. Using this method, plasma concentration and urinary excretion of I were studied after oral administration of I to human volunteers.
建立了一种使用高效液相色谱法（HPLC）结合荧光标记试剂4-（N，N-二甲基氨基磺酰基）-7-N-哌嗪基-2,1,3-苯并恶二唑（DBD-PZ）定量测定人血浆和尿液中HSR-609（I）的简单灵敏方法。化合物I从人血浆和尿液中提取，并在Mukaiyama试剂A（2,2'-二吡啶二硫化物（DPDS）和三苯基膦（TPP）在乙腈中的等摩尔溶液）存在下与DBD-PZ反应进行衍生化。衍生化后，反应混合物通过液液萃取进行净化。共轭物通过离子对HPLC结合荧光检测进行分析。I在血浆中的定量限为0.5 ng/ml，在尿液中的定量限为5 ng/ml。使用该方法，在给人类志愿者口服I后研究了I的血浆浓度和尿排泄情况。
