Ramesh B, Manjula N, Bijargi S R, Sarma V U M, Devi P Sita
Natural Products Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500607, India.
Medicinal Chemistry & Pharmacology Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500607, India.
J Pharm Anal. 2015 Jun;5(3):161-168. doi: 10.1016/j.jpha.2014.11.003. Epub 2014 Dec 2.
Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including (1) liquid-liquid extraction (LLE), (2) solid phase extraction (SPE) and (3) supported liquid extraction (SLE). Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring (MRM) in a positive ion mode with ESI. The transitions monitored were 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification (LLOQ) was 0.2 ng/mL for sitagliptin and 0.1 ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.
比较了三种提取方法用于通过液相色谱-串联质谱法（LC-MS/MS）分析大鼠血浆中西他列汀和辛伐他汀的效率，包括：（1）液-液萃取（LLE）、（2）固相萃取（SPE）和（3）支撑液液萃取（SLE）。不同提取方法对分析物回收率的比较表明，SLE是最佳提取方法。使用离子阱质谱仪通过在正离子模式下的电喷雾电离（ESI）进行多反应监测（MRM）来促进检测。监测的跃迁对于辛伐他汀为441.1→325.2，对于西他列汀为408.2→235.1，对于内标为278.1→260.1。西他列汀的定量下限（LLOQ）为0.2 ng/mL，辛伐他汀为0.1 ng/mL。有效的SLE提供了增强的色谱选择性，从而便于该方法在生物样品常规分析以及药代动力学研究中的潜在应用。
Zotero 插件