适用于人体药理学研究的6-硫鸟嘌呤的反相高效液相色谱分析。

Reversed-phase high-performance liquid chromatography analysis of 6-thioguanine applicable to pharmacologic studies in humans.

作者信息

Andrews P A, Egorin M J, May M E, Bachur N R

出版信息

J Chromatogr. 1982 Jan 8;227(1):83-91. doi: 10.1016/s0378-4347(00)80358-8.

Abstract

6-thioguanine (6TG) and its metabolites were analyzed in human plasma with a reversed-phase high-performance liquid chromatographic methods. 6TG and related compounds were extracted from plasma with an equal volume of 2 N perchloric acid at a 50-100% recovery efficiency. The neutralized extracts were chromatographed on a muBondapak C18 column by two separate isocratic conditions. 6TG, 6-thiouric acid, 6-thioxanthine, 6-thioguanosine, and 6-methylthiouric acid were analyzed with 0.01 M sodium acetate, pH 3.5-10% methanol as the mobile phase and 340 nm for detection. 6-Methylthioguanine and three unknown metabolites were separated with acetate-25% methanol and 310 nm detection. One of the unknowns was identified as 6-methylthioguanosine. External standard calibration was used for quantitation. The 6TG detection limit was 0.8 nmol/ml in plasma.

摘要

采用反相高效液相色谱法分析人血浆中的6-硫鸟嘌呤（6TG）及其代谢产物。用等体积的2N高氯酸从血浆中提取6TG及相关化合物，提取效率为50 - 100%。中和后的提取物在μBondapak C18柱上通过两种不同的等度条件进行色谱分析。以0.01M醋酸钠（pH 3.5）- 10%甲醇为流动相，在340nm波长下检测分析6TG、6-硫尿酸、6-硫黄嘌呤、6-硫鸟苷和6-甲基硫尿酸。以醋酸盐- 25%甲醇为流动相，在310nm波长下检测分离6-甲基硫鸟嘌呤和三种未知代谢产物。其中一种未知物被鉴定为6-甲基硫鸟苷。采用外标法进行定量。血浆中6TG的检测限为0.8nmol/ml。