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本文系统地研究和建立了用反相高效液相色谱法测定生物体液中的地尔硫及其活性代谢物脱乙酰地尔硫的方法。本方法中使用300mm×3.9mm(I.D)Waters不锈钢柱,μ-Bondapak C_(18)(10μm)作固定相,甲醇:缓冲液(0.8％TEMED,pH5.4)60:40(V/V)为流动相。流速为1.3ml/min。检测波长为238nm。以地尔硫(艹卓)的中间体为内标进行定量。本法对地尔硫(艹卓)及脱乙酰地尔硫(艹卓)的检测限均为2ng。血清中最低检测浓度均为5ng/ml。在20、200、1000ng/ml浓度范围内,两者的方法回收率接近100％。天间、天内精密度(CV)均小于5％。用本法对6例服用地尔硫(艹卓)控释片的心绞痛病人进行了临床监测,治疗血浓范围为cmin30～100 ng/ml。
This article systematically studied and established by reversed-phase high performance liquid chromatography in the determination of diltiazem in biological fluids and their active metabolites deacetylase diltiazem method. A 300 mm × 3.9 mm (ID) Waters stainless steel column with μ-Bondapak C_ (18) (10 μm) as the stationary phase and a 60:40 methanol / buffer (0.8% TEMED, pH 5.4) As mobile phase. The flow rate was 1.3 ml / min. The detection wavelength is 238nm. Diltiazem (艹 Zhuo) intermediates as internal standard for quantification. The detection limit of diltiazem and deacetyl diltiazem in this method is 2 ng. The lowest detection serum concentrations were 5ng / ml. At 20,200,1000 ng / ml concentration range, the recovery of the two methods is close to 100%. Days, days, precision (CV) are less than 5%. Six patients with angina pectoris receiving controlled-release diltiazem were monitored by this method. The range of blood concentration was cmin 30-100 ng / ml.