Brode E, Hotz D, Kern R
Methods Find Exp Clin Pharmacol. 1985 Aug;7(8):427-34.
A high pressure liquid chromatographic method with internal analogue standardization for the determination of anipamil in plasma is described. The method comprises extraction from plasma diluted with citrate buffer pH 3 using n-heptane/isoamylalcohol (95/5, v/v), distribution between this organic phase and a methanol/citric acid mixture, and quantification by means of fluorescense detection after HPLC separation using a reverse phase. When using 1 ml plasma the lower limit of detection is 0.2 ng/ml. Under routine conditions the limit of determination is estimated at 1 ng/ml, with higher numbers of replicates and with a predetermined precision limit of 15% concentrations as low as 0.6 ng/ml can be determined reliably. The variation coefficients drop from about 10% in the low range to about 5% at 2 ng/ml or more. The determination of anipamil is not impaired by its N-nor-compound, which is to be expected as metabolite. Neither do other potential metabolites of anipamil with very similar chromatographic behaviour interfere with its quantification.
描述了一种采用内标法的高压液相色谱法测定血浆中阿尼帕米的含量。该方法包括用pH 3的柠檬酸盐缓冲液稀释血浆，然后用正庚烷/异戊醇（95/5，v/v）进行萃取，将该有机相与甲醇/柠檬酸混合物进行分配，最后在反相高效液相色谱分离后通过荧光检测进行定量分析。当使用1 ml血浆时，检测下限为0.2 ng/ml。在常规条件下，测定限估计为1 ng/ml，通过增加重复次数和预定精度限为15%，低至0.6 ng/ml的浓度也能可靠测定。变异系数从低浓度范围的约10%降至2 ng/ml及以上时的约5%。阿尼帕米的N-去甲化合物作为预期的代谢产物，对阿尼帕米的测定没有影响。阿尼帕米其他具有非常相似色谱行为的潜在代谢产物也不会干扰其定量分析。
