【摘要】 目的建立液相色谱-质谱联用（LC-MS）法测定人血清中槲皮素浓度。方法人血清样品经丙酮-甲醇提取,β-葡萄糖醛酸酶水解;采用色谱柱Agilent Poroshell 120 EC C₁₈（50 mm×4.6 mm,2.7μm）,以乙腈（B）和1%甲酸水溶液（A）为流动相,梯度洗脱;流速1.0 m L/min,柱温40℃;电喷雾离子源,单四级杆质谱检测器,选择性负离子监测模式检测（ESI^-）,检测离子质荷比为301.0（槲皮素）,285.1（漆黄素）;测定人血清中槲皮素浓度。结果槲皮素在1²00 ng/m L范围内线性关系良好,相关系数为0.9998;检出限为0.025 ng/m L;日内RSD为4.98%⁸.35%,日间RSD为7.62%⁹.73%;回收率为97.4%¹12.8%（n=8）。结论 LC-MS法灵敏度较高、重复性良好,操作简单、快速,可用于人血清中槲皮素浓度的分析测定。更多还原

【Abstract】 Objective To establish LC-MS method to determine quercetin in human serum. Methods Serum samples were extracted by acetone- methanol and hydrolyzed by β- glucuronidase. The Agilent Poroshell 120 EC C₁₈（ 50 mm × 4. 6 mm,2. 7 μm） was used and acetonitrile（ B） and 1% formic acid（ A） as the mobile phase with gradient elution. Flow rate was 1. 0 m L / min and column temperature 40℃. Liquid chromatography-tandem mass spectrometry（ LC-MS） with electrospray ionization（ ESI^-）was performed in a negative mode and using selective negative ion detection. Detected ion m / z was 301. 1（ quercetin） and 285. 1（ fisetin）. Results The method had good linearity in the concentration ranges of 1- 200 ng / m L. The correlation coefficient（ r） was0. 9998. The detection limits of quercetin was 0. 025 ng / m L. Interday precision（ RSD）was 4. 98%-8. 35%. Intraday precision（ RSD） was 7. 62%-9. 73%. The recoveries of quercetin in serum was 97. 4%-112. 8%. Conclusion The established method is sensitive and reproducible,and can be used in determination of quercetin in human serum.更多还原