摘要
HPLC- DAD同时分析人血浆和尿液中兴奋剂
作者(年代):LailaAbdel Fattah, AmiraM。El-Kosasy, OmarAbd El-Aziz, Naglaa Ebrahim采用zorbaxeclipsehc - c18色谱柱(250mmx4.6mmx5µm)与流动相乙腈,开发了一种高灵敏度的verp - hplc方法,同时分离和定量7种兴奋剂,包括4种利尿剂‘氢氯噻嗪(HCTZ),呋塞米(FUR),吲达帕胺(IDP)和螺内酯(SPIRO)Â′,沙丁胺醇(SAL) â-agonist,合成代谢睾酮(TSE)和皮质类固醇倍他米松(BMS)在加标的人血浆和尿液中:磷酸pH3 (50:50, v/v)在等容条件下,流量为1.0mlmin-1,室温。二极管阵列检测器调整在 ' 225,272, 235, 242和244 '和239 nm,分别定量测定 ' HCTZ, SAL, FUR, IDPandTSE '和 ' SPIRO和BMS '。所研究药物在血浆中的线性范围为100-9000、100-1800、100-5000、200-9000和1000-9000 ng。ml-1分别用于‘HCTZ’和SALÂ′,用于‘FUR’和TSEÂ′,用于IDP,用于SPIROand forms。lod和loq值分别为 ' 31.16、29.99、28.14、29.84、31.98、28.55和250.99 '、 ' 94.42、90.88、85.27、90.42、96.91、86.52和760.58 ' ng ml-1 forHCTZ、SAL、FUR、IDP、TSE、SPIROandBMS;在直接稀释和固相萃取(SPE)后,所研究的药物可以在加标尿液样品中测定,而在最后一种方法(SPE)中,HCTZ和SAL不能测定,因为它们给出了不可重复的结果。Indirectdilutionway;线性范围为150Â→5000→50Â→5000→150Â→1500→100 Â→5000 ng。为ml-1 HCTZ和BMSA,SAL,国内流离失所者和TSEA,一个FURA和SPIROA,分别和一个钟表和LOQs-values39.41,11.98,35.52,12.70,14.11,29.01和40.72和119.42,36.30,107.64,38.48,42.76,87.91和123.39ng。ml-1分别对hctz、SAL、FUR、IDP、TSE、SPIROandBMS进行检测。在SPEmethod; the linearity rangewas 250-3000, 150- 6000 and 150-7000 ng.ml-1 for FUR, IDP and for ÂTSE, SPIRO and BMSÂ, respectively and the ÂLODs and LOQs-values were Â70.11, 39.15, 42.71, 45.91 and 49.01 and 212.45, 118.64, 129.42, 139.12 and 148.52 ng.ml- 1 for FUR, IDP, TSE, SPIROand BMS, respectively. It was shown that SPE is more sensitive, for determination ofFUR, IDP,TSE, SPIROandBMS, than direct dilution(only1:4dilutioncomparedto1:50folddilutionindirectdilution),however, HCTZandSALcould not be determined.
分享这