Bhatt Jignesh, Subbaiah Gunta, Kambli Sandeep, Shah Bhavin, Nigam Samita, Patel Mehul, Saxena Ashish, Baliga Ashok, Parekh Hetal, Yadav Gunvat
Bioanalytical Laboratory, Torrent Research Center, Gandhinagar-382428, Gujarat, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jun 1;852(1-2):115-21. doi: 10.1016/j.jchromb.2007.01.003. Epub 2007 Jan 13.
A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the estimation of rivastigmine in human plasma. Rivastigmine was extracted from human plasma by using solid-phase extraction technique. Zolpidem was used as the internal standard. A Betabasic-8 column provided chromatographic separation of analytes followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 251.20-->206.10, 86.20 for rivastigmine and m/z 308.10-->235.10 for zolpidem. The method involves a rapid solid-phase extraction from plasma, simple isocratic chromatographic conditions and mass spectrometric detection that enables detection at sub-nanogram levels. The proposed method has been validated for a linear range of 0.2-20.0 ng/ml with a correlation coefficient > or =0.9988. The intra-run and inter-run precision and accuracy were within 10.0%. The overall recoveries for rivastigmine and zolpidem were 86.28% and 87.57%, respectively. The total run time was 2.0 min. The developed method was applied for the determination of the pharmacokinetic parameters of rivastigmine following a single oral administration of a 3 mg rivastigmine capsule in 20 healthy male volunteers.
已开发并验证了一种快速灵敏的液相色谱 - 串联质谱法（LC-MS/MS）用于测定人血浆中的 rivastigmine。采用固相萃取技术从人血浆中提取 rivastigmine。唑吡坦用作内标。使用 Betabasic - 8 柱对分析物进行色谱分离，随后用质谱进行检测。rivastigmine 的质量跃迁离子对为 m/z 251.20→206.10、86.20，唑吡坦的质量跃迁离子对为 m/z 308.10→235.10。该方法包括从血浆中快速固相萃取、简单的等度色谱条件和质谱检测，能够在亚纳克水平进行检测。所提出的方法在 0.2 - 20.0 ng/ml 的线性范围内得到验证，相关系数≥0.9988。批内和批间精密度及准确度均在 10.0%以内。rivastigmine 和唑吡坦的总回收率分别为 86.28%和 87.57%。总运行时间为 2.0 分钟。所开发的方法用于在 20 名健康男性志愿者单次口服 3 mg rivastigmine 胶囊后测定 rivastigmine 的药代动力学参数。
