Ramalingam Prakash, Ko Young Tag
College of Pharmacy, Gachon University, Incheon 406-799, South Korea.
College of Pharmacy, Gachon University, Incheon 406-799, South Korea.
J Pharm Biomed Anal. 2016 Feb 5;119:71-5. doi: 10.1016/j.jpba.2015.11.026. Epub 2015 Nov 23.
A rapid, selective, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine resveratrol levels in plasma and brain tissue in mice for supporting pharmacokinetic and brain distribution studies. Analytes were separated using a Sepax BR-C18 analytical column (5μm, 120Å, 1.0×100mm) and eluted using an isocratic elution mobile phase acetonitrile and 0.01% formic acid [60:40, v/v] at a flow rate of 0.1mL/min. Precursor and product ion transitions for analyte resveratrol m/z 226.9>184.8 and curcumin m/z 367.1>148.9 were monitored using triple quadrupole mass spectrometer with multiple reaction monitoring (MRM) in negative ionization mode. The method was validated with respect to accuracy, within- and between-day precision, linearity, limit of quantification, recovery, and matrix effects of analyte. The inter- and intra-day accuracy and precision were within the range of the US Food and Drug Administration (FDA) acceptance criteria, for both matrices. The method was also successfully applied to pharmacokinetic and brain distribution studies of resveratrol after intravenous administration of free resveratrol and resveratrol-loaded solid lipid nanoparticles to mice. The combined use of serial blood sampling, small sample volume, simple extraction, and capillary depletion method drastically improved resveratrol analysis from biological matrices.
建立并验证了一种快速、选择性和灵敏的液相色谱-串联质谱(LC-MS/MS)方法,用于同时测定小鼠血浆和脑组织中白藜芦醇的水平,以支持药代动力学和脑分布研究。使用Sepax BR-C18分析柱(5μm,120Å,1.0×100mm)分离分析物,以0.1mL/min的流速用乙腈和0.01%甲酸[60:40,v/v]的等度洗脱流动相进行洗脱。使用具有多反应监测(MRM)的三重四极杆质谱仪在负离子模式下监测分析物白藜芦醇m/z 226.9>184.8和姜黄素m/z 367.1>148.9的前体离子和产物离子跃迁。该方法在分析物的准确性、日内和日间精密度、线性、定量限、回收率和基质效应方面进行了验证。两种基质的日间和日内准确性和精密度均在美国食品药品监督管理局(FDA)的接受标准范围内。该方法还成功应用于对小鼠静脉注射游离白藜芦醇和载白藜芦醇固体脂质纳米粒后白藜芦醇的药代动力学和脑分布研究。连续采血、小样本量、简单提取和毛细血管耗竭法的联合使用极大地改善了生物基质中白藜芦醇的分析。