摘要
本法用ＷａｔｅｒｓＢａｓｅｌｉｎｅ８１０色谱工作站，Ｗａｔｅｒｓ径向加压柱（Ｎｏｖａ－ＰａｋＣ＿（１８）８ｍｍ×１０ｃｍ，４μｍ），检测波长ＵＶ２３８ｎｍ，流动相为甲醇－水－二氯甲烷－０．１ｍｏｌ／Ｌ醋酸铵（６４：２３．５：２．５：１０），流速：２．０ｍｌ／ｍｉｎ；血样用混合溶剂一次提取，地尔硫和去乙酰地尔硫的提取回收率分别为８５．２％、８２．３％，平均方法回收率分别为９９．６％、１０１．１％，最低检测浓度均为５ｎｇ／ｍｌ。
Diltiazem(DZ)is a benzothiazepine derivative with calcium-channel activity.It’s major metabolite is deacetyldiltiazem(DADZ)that showing pharmacological activity,The paper introduces a new HPLC methods for simultaneous quantitation of DZ and DADZ.Experiments were performed on Waters Baseline 810 HPLC system。A100mm × 8mm ID Waters radial compression modual(RCM)column was packed with 4μm Nova-Pak C_(18).The mobile phase was consisted of methanol-water-dichloromethane-0.1mol/L ammonium acetate solution(64:23.5:2.5:10)with the flow rate of 2.0ml/min,Haloperidoli was used as internal standard.1ml plasma sample was alkalinized with 0.5ml borate buffer(pH9.0)and 200ng of internal standard and 5ml of ether-n-butanol(95:5)were then added.The tubes were shaken for 3min and then centrifuged for 10min at 4000rlmin. The orgauic phase was transferred to another tubes,then vaporized by nitrogen. The residual reconstituted with 30μl of 5m mol/L H_2SO_4.20μl of the sample solution were injected for HPLC. The standard curves of plasma sample with linear range over the concentration 10～200ng/ml of DZ and DADZ,respectively were observed. The recoveries of DZ and DADZ were 99.6%and 10l.1%,respectively.Extraction efficiency of DZ and DADZ were 85.3%and 82.3%,respectively.
出处
《药物分析杂志》
CAS
CSCD
北大核心
1995年第6期20-21,共2页
Chinese Journal of Pharmaceutical Analysis
