使用短链烷基硅烷醇去活柱，通过高效液相色谱法测定血浆中的地尔硫䓬及其两种代谢物。
High-performance liquid chromatographic determination of diltiazem and two of its metabolites in plasma using a short alkyl chain silanol deactivated column.
作者信息
Rutledge D R, Abadi A H, Lopez L M, Beaudreau C A
机构信息
College of Pharmacy, University of Florida, Gainesville 32610.
出版信息
J Chromatogr. 1993 May 19;615(1):111-6. doi: 10.1016/0378-4347(93)80296-g.
A simple and reproducible method for the determination of diltiazem and its two major metabolites, demethyl- and deacetyldiltiazem, is presented using a new column containing a short alkyl chain silanol deactivated support. This method involves the extraction of alkalinized plasma with a hexane-isopropanol mixture (95:5, v/v) followed by back-extraction into 5 mM sulfuric acid. Reversed-phase liquid chromatography is used with ultraviolet detection at 237 nm over a concentration range of 20-400 ng/ml for the compounds. Imipramine is used as the internal standard. Within-day and between-day coefficients of variation are less than 10%. The lower limits of detection are 4, 2 and 4 ng/ml for diltiazem, deacetyl- and demethyldiltiazem, respectively. Samples can be stored for up to thirty days with no significant degradation. The assay has clinical applicability.
本文介绍了一种简单且可重复的方法，用于测定地尔硫䓬及其两种主要代谢产物去甲基地尔硫䓬和去乙酰地尔硫䓬，该方法使用了一种含有短烷基链硅烷醇钝化载体的新型色谱柱。该方法包括用己烷 - 异丙醇混合物（95:5，v/v）萃取碱化血浆，然后反萃取到5 mM硫酸中。采用反相液相色谱法，在237 nm处进行紫外检测，化合物的浓度范围为20 - 400 ng/ml。以丙咪嗪作为内标。日内和日间变异系数均小于10%。地尔硫䓬、去乙酰地尔硫䓬和去甲基地尔硫䓬的检测下限分别为4、2和4 ng/ml。样品可保存长达30天而无明显降解。该测定方法具有临床适用性。
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