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目的建立比格犬血浆中烟酸及其代谢物烟尿酸的RP-HPLC测定方法。方法血浆样品用甲醇沉淀蛋白,上清液氮气流吹干,残留物用流动相复溶后分析,以富马酸为内标。色谱柱:Diamon-sil C18柱(4.6 mm×200 mm,5μm),流动相:甲醇-0.04 mol.L-1四丁基溴化铵溶液(体积比为30∶70),流速:1.0 mL.min-1,柱温:20℃,检测波长:262 nm。结果烟酸在0.20~80.0 mg.L-1质量浓度内线性关系良好,高、中、低3种质量浓度QC样品的日内、日间RSD均小于8.0%,提取回收率在90.0%~97.8%之间;烟尿酸在0.10~5.0 mg.L-1浓度范围内线性关系良好,高、中、低3种浓度QC样品的日内、日间RSD均小于9.1%,提取回收率在95.9%~99.5%之间。结论该方法适用于血浆中烟酸和烟尿酸浓度的测定和药动学研究。
Objective To establish a method for the determination of nicotinic acid and its metabolite nicotinic acid in Beagle dog plasma by RP-HPLC. Methods The plasma samples were precipitated with methanol and the supernatant was air-dried with a nitrogen stream. The residue was reconstituted with a mobile phase and analyzed with fumaric acid as an internal standard. Column: Diamon-sil C18 column (4.6 mm × 200 mm, 5 μm) with a mobile phase of methanol-0.04 mol·L-1 tetrabutylammonium bromide (volume ratio of 30:70) at a flow rate of 1.0 mL. min-1, column temperature: 20 ℃, detection wavelength: 262 nm. Results The niacin showed good linearity in the concentration range of 0.20 ~ 80.0 mg.L-1. The RSDs of day, day and day of high, medium and low concentration of QC were less than 8.0% and the recoveries ranged from 90.0% to 97.8% . The concentrations of niacin in the range of 0.10-5.0 mg · L-1 showed good linearity. The daily RSD and RSD of high, medium and low concentrations of QC were all less than 9.1% and the extraction recoveries ranged from 95.9% to 99.5 %between. Conclusion The method is suitable for the determination of niacin and uric acid in plasma and pharmacokinetic study.