Kumar Avinash, Devaraj V C, Giri Kalpesh C, Giri Sanjeev, Rajagopal Sriram, Mullangi Ramesh
Drug Metabolism and Pharmacokinetics, Jubilant Biosys Ltd, Industrial Suburb, Yeshwanthpur, Bangalore-560022, India.
Biomed Chromatogr. 2012 Dec;26(12):1464-71. doi: 10.1002/bmc.2717. Epub 2012 Feb 21.
A highly sensitive, rapid assay method has been developed and validated for the estimation of nobiletin in rat plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive-ion mode. The assay procedure involves extraction of nobiletin and citalopram (internal standard, IS) from rat plasma with liquid-liquid extraction. Chromatographic separation was achieved using an isocratic mobile phase (0.2% formic acid-acetonitrile, 20:80, v/v) at a flow rate of 0.6 mL/min on an Atlantis dC₁₈ column (maintained at 40 ± 1 °C) with a total run time of 2.0 min. The MS/MS ion transitions monitored were 403.2 → 373.0 for nobiletin and 325.2 → 109.0 for IS. Method validation was performed as per Food and Drug Administration guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.05 ng/mL and the linearity range extended from 0.05 to 51.98 ng/mL. The intra- and inter-day precisions were in the range of 1.96-14.3 and 6.21-12.1, respectively.
已开发并验证了一种高灵敏度、快速的检测方法，用于采用液相色谱-串联质谱联用（正离子模式下的电喷雾电离）测定大鼠血浆中的川陈皮素。该检测程序包括通过液-液萃取从大鼠血浆中提取川陈皮素和西酞普兰（内标，IS）。在Atlantis dC₁₈柱（保持在40±1℃）上，以0.6 mL/min的流速使用等度流动相（0.2%甲酸-乙腈，20:80，v/v）进行色谱分离，总运行时间为2.0分钟。监测的MS/MS离子跃迁对于川陈皮素为403.2→373.0，对于内标为325.2→109.0。按照美国食品药品监督管理局的指南进行方法验证，结果符合验收标准。达到的定量下限为0.05 ng/mL，线性范围从0.05扩展至51.98 ng/mL。日内和日间精密度分别在1.96 - 14.3和6.21 - 12.1范围内。
