Silva Lara C, Oliveira Lina S O B, Mendes Gustavo D, Garcia Gabriel, Pereira Alberto Dos Santos, De Nucci Gilberto
Faculty of Medical Sciences, State University of Campinas-UNICAMP, P.O. Box 6111, Campinas, SP, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Mar 7;832(2):302-6. doi: 10.1016/j.jchromb.2005.12.027. Epub 2006 Feb 7.
Isosorbide 5-mononitrate (5-ISMN) is an organic nitrate widely used for its vasodilating properties in the treatment of angina pectoris. In the present study, an efficient, sensitive, robust method was developed for the determination and quantification of isosorbide 5-mononitrate, in human plasma, by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS), using photospray ionization. Isosorbide 5-mononitrate was extracted from 0.5 mL human plasma by liquid-liquid extraction (LLE). The method had a chromatographic run of 2.0 min using a C(8) analytical column (100 mm x 2.1 mm i.d.) and the linear calibration curve over the range was linear from 20 to 2000 ng mL(-1) (r(2)>0.995). The between-run precision, based on the relative standard deviation replicate quality controls, was 7.9% (60 ng mL(-1)), 5.2% (300 ng mL(-1)) and 7.0% (1800 ng mL(-1)). The between-run accuracy was 94.9%, 94.1% and 88.8% for the above-mentioned concentrations, respectively. The method herein described was employed in a bioequivalence study of two tablet formulations of isosorbide 5-mononitrate 40 mg.
5-单硝酸异山梨酯（5-ISMN）是一种有机硝酸盐，因其血管舒张特性而被广泛用于治疗心绞痛。在本研究中，开发了一种高效、灵敏、稳健的方法，采用液相色谱-串联质谱法（LC-MS/MS）结合光喷雾电离技术，用于测定和定量人血浆中的5-单硝酸异山梨酯。通过液-液萃取（LLE）从0.5 mL人血浆中提取5-单硝酸异山梨酯。该方法使用C(8)分析柱（100 mm×2.1 mm内径）进行2.0分钟的色谱运行，线性校准曲线在20至2000 ng mL(-1)范围内呈线性（r(2)>0.995）。基于相对标准偏差重复质量控制的批间精密度分别为7.9%（60 ng mL(-1)）、5.2%（300 ng mL(-1)）和7.0%（1800 ng mL(-1)）。上述浓度的批间准确度分别为94.9%、94.1%和88.8%。本文所述方法用于40 mg 5-单硝酸异山梨酯两种片剂剂型的生物等效性研究。
