尿液中利尿剂、丙磺舒、咖啡因、匹莫林的固相提取和HPLC初筛分析

SOLID-PHASE EXTRACTION AND RP-HPLC SCREENING ROCEDURE FOR DIURETICS,PROBENECID,CAFFEINE AND PEMOLINE IN URINE

利尿剂广泛应用于治疗高血压和水肿。近年来,利尿剂在体育竞赛中被滥用。丙磺舒是一种抗痛风药,因该药主要在肾脏排泄,竞争性的抑制了其它药物(如甾体类药物)的排泄,为此服用过甾体类药物的运动员用它来帮助逃避药物检查。国际奥委会在1988年奥运会上正式禁用利尿剂和丙磺舒。咖啡因和匹莫林属中枢兴奋剂,因其挥发性差,气相检测困难,因此也同利尿剂一起分析。

A solid-phase extraction and reversed phase high performance liquid chromatographic method(RP-HPLC) was developed for the rapid determination of 13 diuretics (bel- onging to five different pharmacological groups) ,probenecid, caffeine and pemoline in urine. Two ml urine sample was first adsorbed on a XAD-2 column, then eluted with ether--ethyl acetate(l: 1). The eluate was evaporated to dryness and reconstituted in methanol. The methanolic solution was injected into a HP LiChrosorb RP-18 column, using phosphate buffer (pH 3) and acetonitrile as the mo- bile phase and monitored at 216 nm, 230 nm, and 275 nm on a diode array ultraviolet detector. The extraction recoveries of 16 drugs were above 75%. The limits of detection ranged from 0. 3～3.0 μg/ml of urine. All drugs were separately administered to healthy volunteers, positive urine samples were collected, and urinary excretion--time curves of some drugs were reported.