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目的建立人血浆中烟酸及其代谢物的高效液相色谱-质谱联用(HPLC-MS/MS)测定法。方法血浆样品加乙腈沉淀蛋白,取上清液挥干,用流动相溶解,二氯甲烷反洗后进样分析。使用Genimi C18柱(50×3.00mm,3μm),柱温35℃,流动相为0.1%乙酸水溶液∶甲醇∶异丙醇(98:1:1),流速为0.2 mL/min,以正离子MRM模式检测,烟酸、烟酰胺、烟脲酸和内标6-甲基烟酸的检测离子对质荷比(m/z)分别为124.1→80.0、123.1→80.0、181.1→135.0和138.1→92.0。结果烟酸线性范围为1.25~320μg/L,烟酰胺和烟脲酸线性范围均为1.25~1280μg/L,最低检测限均为1.25μg/L,日内和日间RSD均小于9%,方法回收率为89%~105%。结论该法具有快速、灵敏、准确、简便等特点,适用于人血浆烟酸浓度测定及药代动力学和生物利用度研究。
Objective To establish a high performance liquid chromatography-mass spectrometry (HPLC-MS / MS) method for determination of niacin and its metabolites in human plasma. Methods Plasma samples were precipitated with acetonitrile and the supernatant was evaporated to dryness, dissolved in mobile phase and back-washed with methylene chloride. A Genimi C18 column (50 × 3.00mm, 3μm) was used. The column temperature was 35 ℃ and the mobile phase consisted of 0.1% aqueous acetic acid: methanol: isopropanol (98: 1: 1) The detection mass ratios (m / z) of niacin, nicotinamide, tranexamic acid and 6-methylnicotinic acid were 124.1 → 80.0, 123.1 → 80.0, 181.1 → 135.0 and 138.1 → 92.0, respectively. Results The linear range of niacin was 1.25-320 μg / L. The linear range of niacinamide and tranexamic acid were 1.25-1280 μg / L with the lowest detection limit of 1.25 μg / L. The RSDs were both less than 9% during the day and the day. The rate of 89% to 105%. Conclusion The method is fast, sensitive, accurate and simple. It is suitable for the determination of niacin in human plasma and its pharmacokinetics and bioavailability.