AbuRuz S, Millership J, Heaney L, McElnay J
Clinical and Practice Research Group, School of Pharmacy, Queens University Belfast, 97 Lisburn Road, Belfast BT9 7BL, UK.
J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Dec 25;798(2):193-201. doi: 10.1016/j.jchromb.2003.09.044.
This article describes the development and validation of a simple solid phase extraction (SPE) and HPLC method for the extraction and the specific determination of prednisolone and hydrocortisone (cortisol) in both plasma and urine using one washing step with Oasis hydrophilic lipophilic balanced (HLB) cartridges (1 ml/30 mg, 30 microm). Recoveries of prednisolone and cortisol from plasma and urine exceeded 82%. The limit of quantification (LOQ) in plasma and urine was 9.9 and 6.7 ng/ml for cortisol, respectively, and 11.6 and 8.0 ng/ml for prednisolone, respectively. The intraday and interday precision (measured by CV%) for both prednisolone and cortisol in both plasma and urine was always less than 7%. The accuracy (measured by relative error %) for both prednisolone and cortisol in both plasma and urine was always less than 8%. The advantages of the developed method are the use of a one step washing SPE utilising HLB cartridges which do not suffer the drying out problems of conventional SPE cartridges and the time saving when compared with solvent extraction (SE), in addition to the simultaneous determination of prednisolone and cortisol in both plasma and urine.
本文介绍了一种简单的固相萃取(SPE)和高效液相色谱(HPLC)方法的开发与验证,该方法使用Oasis亲水亲脂平衡(HLB)小柱(1 ml/30 mg,30 µm)进行一步洗涤,用于血浆和尿液中泼尼松龙和氢化可的松(皮质醇)的萃取和特异性测定。泼尼松龙和皮质醇从血浆和尿液中的回收率超过82%。血浆和尿液中皮质醇的定量限(LOQ)分别为9.9和6.7 ng/ml,泼尼松龙分别为11.6和8.0 ng/ml。血浆和尿液中泼尼松龙和皮质醇的日内和日间精密度(以CV%衡量)始终小于7%。血浆和尿液中泼尼松龙和皮质醇的准确度(以相对误差%衡量)始终小于8%。所开发方法的优点包括使用一步洗涤的SPE,利用HLB小柱,其不存在传统SPE小柱的干涸问题,与溶剂萃取(SE)相比节省时间,此外还能同时测定血浆和尿液中的泼尼松龙和皮质醇。