柱切换HPLC法测定血浆和尿中卡托普利浓度

卡托普利先经衍生化形成具有紫外吸收的衍生物,然后用6%的高氯酸去蛋白,取上清液直接进样。以μBoundapak C₁₈(37～50μm)作为预处理柱(5cm×O.5cm,ID),对样品进行自动浓缩净化处理,预处理流动相为0.2%醋酸溶液。分析柱(15cm×O.5cm,ID)固定相为YWG-C₁₃,10μm,流动相为乙晴-水-醋酸(35:65:0.4)。UV 260nm检测。血浆和尿样测定的线性范围分别为20～1000ng/ml和10～200μg/ml,血浆中最低检测浓度约为10ng/ml。方法的平均回收率分别为103.2%(血浆)和99.5%(尿样),日内及日间变异均小于10%。

DETERMINATION OF CAPTOPRIL IN PLASMA AND URINE BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY WITH COLUMN SWITCHING

A rapid and sensitive column-switching high performance liquid chromatographic procedures was described for determination of captopril in plasma and urine. p-Bromophenacyl bromide, a derivatizing reagent, was added to the plasma and urine samples to form an adduct which showed ultraviolet absorbing properties. After that, the urine sample was injected directly and for plasma the protein was removed with 6% of perchloride before injection. The column-switching system was equipped with a pre-column of 5 cm x 0.5 cm ID, packed with mu Boundapak C18, 37-50 microns, and an analytical column of 15 cm x 0.5 cm ID, packed with YWG-C18, 10 microns. After washing out the impures from pre-column with 0.2% acetic acid the retained substances were eluted into analytical column with acetonitrile-water-acetic acid (35:65:0.4). Captopril was detected at 260 nm. The method was linear within 20-1000 ng/ml for plasma and 10-200 micrograms/ml for urine. The recovery averaged 103.2% and 99.5% for plasma and urine, respectively. The coefficient variations were all less than 10%.