Konda Ravi Kumar, Chandu Babu Rao, Challa B R, Kothapalli Chandrasekhar B
Hindu College of Pharmacy, Amaravathi Road, Guntur, Andhra Pradesh 522002, India.
Jawaharlal Nehru Technological University, Anantapur, Andhra Pradesh 515002, India.
J Pharm Anal. 2012 Oct;2(5):342-349. doi: 10.1016/j.jpha.2012.04.001. Epub 2012 May 11.
The most suitable bio-analytical method based on liquid-liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-C mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm×50 mm, 3.5 μm) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The total run time was 3.0 min. The proposed method has been validated with the linear range of 5-12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3%-2.9% and 1.6%-2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-C mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition.
已开发并验证了基于液-液萃取的最适合生物分析方法，用于定量测定人血浆中的雷沙吉兰。甲磺酸雷沙吉兰-C用作雷沙吉兰的内标。Zorbax Eclipse Plus C18（2.1mm×50mm，3.5μm）色谱柱对分析物进行色谱分离，随后采用质谱检测。该方法采用简单的等度色谱条件，并使用API-4000系统在正离子模式下进行质谱检测。总运行时间为3.0分钟。所提出的方法已在雷沙吉兰5-12000 pg/mL的线性范围内得到验证。雷沙吉兰的批内和批间精密度值分别在1.3%-2.9%和1.6%-2.2%以内。雷沙吉兰和甲磺酸雷沙吉兰-C类似物的总回收率分别为96.9%和96.7%。该验证方法已成功应用于空腹条件下人体志愿者的生物等效性和药代动力学研究。
