Sturm E, Junker A
Byk Gulden Pharmaceuticals, Konstanz, F.R.G.
J Chromatogr. 1988 Aug 19;430(1):43-51. doi: 10.1016/s0378-4347(00)83132-1.
A method for determining telenzepine in human serum is described. Analytes are obtained from alkalinized serum by extraction of the drug using reversed-phase octadecylsilane-bonded silica cartridges. Telenzepine and a desmethyl analogue added to serum as internal standard are retained on the C18 cartridge and recovered by elution with methanol. The gas chromatographic properties of telenzepine and the internal standard are improved by a two-step derivatization involving a benzodiazepinone-benzimidazole rearrangement and simultaneous formation of a methyl ester function. The processed extract is analysed by gas chromatography-mass spectrometry with selected-ion monitoring. Quantification is linear over the range 2-40 ng/ml. Inter-day precision is within 7%, except at the detection limit of 2 ng/ml (16%). Application of this assay to routine analysis is limited by the extensive sample pretreatment essential for derivatization of telenzepine.
描述了一种测定人血清中替仑西平的方法。通过使用反相十八烷基硅烷键合硅胶柱从碱化血清中提取药物来获得分析物。作为内标添加到血清中的替仑西平和去甲基类似物保留在C18柱上，并通过用甲醇洗脱回收。通过两步衍生化改善替仑西平和内标的气相色谱性质，该衍生化涉及苯二氮卓酮 - 苯并咪唑重排并同时形成甲酯官能团。通过气相色谱 - 质谱联用选择离子监测对处理后的提取物进行分析。定量在2 - 40 ng/ml范围内呈线性。日间精密度在7%以内，但检测限为2 ng/ml时除外（16%）。该测定法在常规分析中的应用受到替仑西平衍生化所需的广泛样品预处理的限制。
