HPLC Group, Analytical Chemistry Division, Discovery Laboratory, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500607, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jul 1;879(21):1911-6. doi: 10.1016/j.jchromb.2011.05.017. Epub 2011 May 20.
A simple and rapid reverse polar ionic LC method was developed and validated for simultaneous separation and determination of mirtazapine, an antidepressant drug, and its main metabolite N-desmethyl mirtazapine using fluorescence and polarimetric detectors connected in series. The chromatographic separation was achieved on Chirobiotic V column packed with vancomycin as a stationary phase in an isocratic mode of elution of methanol:glacial acetic acid:anhydrous triethyl amine (100:0.2:0.1, v/v/v) as a mobile phase. The compounds were detected by their excitation at 290nm and emission at 370nm using fluorescence detector while the optical rotation (+/-) of the enantiomers was identified by polarimetric detector. The analytes were extracted from rat plasma by precipitation of proteins and the average yield was 88-111% for mirtazapine and 85-123% for N-desmethyl mirtazapine. The method was linear over the concentration range of 20-5000ng/mL. The method was successfully applied on rat plasma spiked with the enantiomers of mirtazapine and N-desmethyl mirtazapine.
建立并验证了一种简单、快速的反相离子对 HPLC 方法，用于同时分离和测定抗抑郁药米氮平及其主要代谢物 N-去甲基米氮平。采用荧光和圆二色性检测器串联，米氮平和 N-去甲基米氮平在万古霉素手性柱上以甲醇：冰醋酸：无水三乙胺（100:0.2:0.1，v/v/v）为流动相进行等度洗脱。用荧光检测器在 290nm 激发、370nm 发射波长下检测化合物，用圆二色性检测器检测对映体的旋光（+/-）。米氮平和 N-去甲基米氮平采用蛋白沉淀法从大鼠血浆中提取，平均回收率为 88-111%和 85-123%。该方法在 20-5000ng/mL 浓度范围内呈线性。该方法成功应用于大鼠血浆中米氮平和 N-去甲基米氮平对映体的测定。
