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血浆中泼尼松和泼尼松龙的液相色谱同步测定

Simultaneous liquid-chromatographic determination of prednisone and prednisolone in plasma.

作者信息

Cheng M H, Huang W Y, Lipsey A I

机构信息

Clinical Laboratory, Childrens Hospital, Los Angeles, CA 90027.

出版信息

Clin Chem. 1988 Sep;34(9):1897-9.

PMID:3416442
Abstract

This high-performance liquid-chromatographic (HPLC) method for simultaneous determination of prednisone and its metabolite, prednisolone, in plasma is a modification of the method of Frey et al. (Clin Chem 1979;25:1944-7). Heparinized plasma (1.0 mL) with 0.1 mL of internal standard solution (11-deoxy-17-hydroxycorticosterone, 2 mg/L) is extracted with 7.0 mL of dichloromethane, then washed sequentially with 0.1 mol/L HCl, 0.1 mol/L NaOH, and deionized water, 2.0 mL each. The extract is evaporated and the residue reconstituted with 75 microL of mobile phase, methanol/H2O (40/60 by vol). Thirty microliters of this is injected onto a reversed-phase C6 column, which is eluted at 1.4 mL/min. Analytical recoveries of prednisone and prednisolone were 94-98% and 102-106%, respectively. Day-to-day precision (CV) was 3.8% for prednisone, 6.1% for prednisolone. We encountered no interference from the 21 other steroids and 25 drugs tested. This method is simple, accurate, and precise.

摘要

这种用于同时测定血浆中泼尼松及其代谢物泼尼松龙的高效液相色谱(HPLC)方法是对Frey等人(《临床化学》1979年;25:1944 - 1947)方法的改进。将1.0 mL肝素化血浆与0.1 mL内标溶液(11 - 脱氧 - 17 - 羟皮质酮,2 mg/L)用7.0 mL二氯甲烷萃取,然后依次用0.1 mol/L盐酸、0.1 mol/L氢氧化钠和去离子水各2.0 mL洗涤。提取物蒸发,残渣用75 μL流动相甲醇/水(体积比40/60)复溶。取30 μL注入反相C6柱,以1.4 mL/min的流速洗脱。泼尼松和泼尼松龙的分析回收率分别为94% - 98%和102% - 106%。泼尼松的日间精密度(CV)为3.8%,泼尼松龙为6.1%。我们在测试的其他21种类固醇和25种药物中未遇到干扰。该方法简单、准确且精密。

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Simultaneous liquid-chromatographic determination of prednisone and prednisolone in plasma.血浆中泼尼松和泼尼松龙的液相色谱同步测定
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