Sun Xiaohong, Li Xiaoqin, Cai Shuang, Qin Feng, Lu Xiumei, Li Famei
Department of Analytical Chemistry, Shenyang Pharmaceutical University, Shenyang 110016, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Feb 1;846(1-2):323-8. doi: 10.1016/j.jchromb.2006.08.022. Epub 2006 Sep 7.
A novel, selective and sensitive high performance liquid chromatography-mass spectrometric (HPLC-MS) method has been developed for the determination of isosorbide 5-mononitrate (5-ISMN) in human plasma. With acetaminophen as internal standard, sample pretreatment involved one-step extraction with diethyl ether of 0.5 mL plasma. Analysis was performed on an ACQUITY UPLC BEH C(18) column (100 mm x 2.1mm, 1.7 microm) with mobile phase consisting of acetonitrile-water (20:80, v/v). The detection was carried out by means of electrospray ionization mass spectrometry in negative ion mode with selected ion recording (SIR). Standard curves were linear (r(2)> or =0.99) over the concentration range of 1.04-1040 ng/mL. The lower limit of quantification (LLOQ) was 1.04 ng/mL. The intra- and inter-day precisions (RSDs) were less than 8.6% and 13.4%, respectively, and the accuracy (RE) was within +/-0.45%. The method herein described was fully validated and successfully applied to the pharmacokinetic study of 5-ISMN in compound extended-release tablets in 18 healthy male volunteers after oral administration.
已开发出一种新颖、选择性好且灵敏的高效液相色谱-质谱联用（HPLC-MS）方法，用于测定人血浆中的5-单硝酸异山梨酯（5-ISMN）。以对乙酰氨基酚为内标，样品预处理包括用0.5 mL乙醚对血浆进行一步萃取。分析在ACQUITY UPLC BEH C(18)柱（100 mm×2.1mm，1.7μm）上进行，流动相为乙腈-水（20:80，v/v）。采用电喷雾电离质谱在负离子模式下进行选择离子记录（SIR）检测。标准曲线在1.04 - 1040 ng/mL浓度范围内呈线性（r(2)≥0.99）。定量下限（LLOQ）为1.04 ng/mL。日内和日间精密度（RSDs）分别小于8.6%和13.4%，准确度（RE）在±0.45%以内。本文所述方法经过充分验证，并成功应用于18名健康男性志愿者口服复方缓释片后5-ISMN的药代动力学研究。
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