Development of Cinnarizine Analysis Method in Human Blood Plasma Using UPLC MS/MS Uswatun Hasanah(a*), Ade Heri Mulyati(a), Siti Amelia Zuchrofah(b)
a) Universitas Pakuan, Bogor, Indonesia
Jalan Pakuan, Baranangsiang, Bogor, Indonesia.
*)uswatun.hasanah[at]unpak.ac.id
b) PT. Equilab International
Jalan Rumah Sakit Fatmawati Persil 33 Jakarta Selatan, Indonesia
Abstract
Cinnarizine is a generic drug with properties as an antihistamine and a sedative that produces significant effects for preventing or treating motion sickness. Generic drugs have the same quality and pharmacological response as patent drugs, so it is necessary to do a BA/BE test to control the quality of generic drugs. This research has optimum conditions with the composition of the mobile phase ammonium acetate 5mM pH 4.5: acetonitrile (35:65) with a flow rate of 0.2 mL/min. and an injection volume of 10 L, extraction using tert-butyl methyl ether (TBME) with a volume of 3 mL. The standard molecular mass of cinnarizine is 369.17 m/z with 167.02 m/z fragmentation. The standard molecular mass of loratadine is 383.07 m/z with 337.07 m/z fragmentation. Validation of the analytical method showed that human blood plasma blanks gave a response but were still included in the selectivity test^s acceptance criteria. The carry-over test indicates that there is no carry-over in the injection. LLOQ test shows analyte signal >5x blank signal. The linearity of the calibration curve is higher than 0.99. The accuracy test (% different) and precision (% RSD) are samples with low, medium, high and highest concentrations of \pm 15%, while the lowest concentration of \pm 20%. The dilution measurement met the requirements for percent different \pm 15% for and dilutions. Standard solutions are stable at storage temperatures for up to 18 days. Blood plasma samples containing cinnarizine were stable at room temperature for up to 6 hours, at storage temperature for 17 days and frozen for four cycles. The validation of the analytical method in this study refers to the EMA guidelines.
