Zhang Pingping, Sun Yantong, Shi Guobing, Sui Yin, Li Qiuying, Tang Yunbiao, Gu Jingkai
Department of Pharmacy, General Hospital of Shenyang Military Area Command, No. 83, Wenhua Road, Shenhe District, Shenyang 110840, China.
Research Center for Drug Metabolism, School of Life Sciences, Jilin University, Changchun 130012, China.
Int J Anal Chem. 2015;2015:212437. doi: 10.1155/2015/212437. Epub 2015 Aug 5.
Our paper aimed to develop rapid, sensitive, and specific LC-MS/MS method for the quantification of niacin (NA) and its metabolite nicotinuric acid (NUA) in human plasma. Following protein precipitation with acetonitrile, the NA, NUA, and internal standard (5-fluorouracil) were separated on a Zorbax 300SB-C8 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of methanol-2 mM ammonium acetate (3 : 97, v/v) at a flow rate of 1 mL/min (split 1 : 1). A tandem mass spectrometer equipped with electrospray ionization source was used as the detector and operated in negative ion mode. The linear concentration ranges of the calibration curves were 5-800 ng/mL for NA and NUA. The intra-assay RSD for quality control (QC) samples were from 5.0% to 8.7% for NA, and 5.5% to 7.6% for NUA. The interassay RSD for QC samples were from 2.8% to 9.4% for NA, and 3.7% to 5.8% for NUA. The relative errors for QC samples were from -2.2% to 2.3% for NA, and -0.6% to 3.2% for NUA. The method was successfully applied to the investigation of the pharmacokinetic profiles of NA, NUA in human after single dose administration of Niacin extended-release/Simvastatin tablet (500 mg/10 mg).
我们的论文旨在开发一种快速、灵敏且特异的液相色谱-串联质谱法（LC-MS/MS），用于定量测定人血浆中的烟酸（NA）及其代谢产物烟尿酸（NUA）。用乙腈进行蛋白沉淀后，NA、NUA和内标（5-氟尿嘧啶）在Zorbax 300SB-C8柱（250 mm×4.6 mm，5μm）上分离，流动相为甲醇-2 mM醋酸铵（3∶97，v/v），流速为1 mL/min（分流比1∶1）。配备电喷雾电离源的串联质谱仪用作检测器，以负离子模式运行。校准曲线的线性浓度范围为NA和NUA均为5-800 ng/mL。质量控制（QC）样品的批内相对标准偏差（RSD），NA为5.0%至8.7%，NUA为5.5%至7.6%。QC样品的批间RSD，NA为2.8%至9.4%，NUA为3.7%至5.8%。QC样品的相对误差，NA为-2.2%至2.3%，NUA为-0.6%至3.2%。该方法成功应用于单次服用烟酸缓释/辛伐他汀片（500 mg/10 mg）后人血浆中NA、NUA药代动力学特征的研究。
