Liquid chromatography tandem mass spectrometry method for the quantification of rimonabant, a CB1 receptor antagonist, in human plasma

Abstract

A sensitive high-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the quantification of rimonabant in human plasma. Following liquid-liquid extraction, the analytes were separated using an isocratic mobile phase on a reverse-phase column and analyzed by MS/MS in the multiple reaction monitoring mode using the respective (M+H)+ ions, m/z 463-363 for rimonabant and m/z 408-235 for the internal standard. The assay exhibited a linear dynamic range of 0.1-100 ng/mL for rimonabant in human plasma. The lower limit of quantification was 0.1 ng/mL with a relative standard deviation of less than 6%. With dilution integrity up to 10-fold, the upper limit of quantification was extendable up to 1000 ng/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 2.0 min for each sample made it possible to analyze more than 250 human plasma samples per day. The validated method was successfully used to analyze human plasma samples for application in pharmacokinetic studies.

Validation of bioanalytical LC–MS/MS assays: Evaluation of matrix effects

“…However, some authors only investigated the absolute matrix effect and did not evaluate the effect of matrices from different sources [31,[58][59][60][61][62][63][64][65][66][67][68]. Cao et al [62] have quantified methyl protodioscin, a natural furostanol saponin with antitumor activity, in rat plasma after PPT.…”

Determination of rimonabant in human plasma and hair by liquid chromatography–mass spectrometry

“…1A2 and B2), as in the method of McCulloch et al [24]. In the previously described method of Niragi et al [23], sitagliptin was used, but provided an extraction recovery 17.8% lower than the one of rimonabant. Fig.…”

“…Nirogi et al [23] reported an LC-MS/MS method for quantification of rimonabant in a short range of concentration (0.1-100 ng/mL) from 200 L of plasma, while therapeutic concentrations range from about 100 to 200 ng/mL. McCulloch et al [24] also reported quantification of rimonabant in plasma, but after a single protein precipitation from 200 L of plasma.…”

A Simple and Convenient Method for Simultaneous Determination of Four Major Species of Illegal Additives in Slimming Health Food

“…The orlistat is generally determined by a HPLC-UV method, [16,17] the sibutramine can be detected by the LS=MS, or HPLC-UV method, [18] rimonabant is detected by the HPLC-MS method. [19][20][21][22] Maybe because cetilistat is a newly developed medicine, which has not been come into market, the detection method has not been described in data. Beside, these seldom reported methods are complicated, time consuming, and need different analytical instruments.…”