FENTI INDAH NIRWANA, 051514153015 (2018) PENGEMBANGAN METODE PENETAPAN KADAR VITAMIN B12 DALAM SEDIAAN MULTIVITAMIN BENTUK PADAT SECARA LC-MS/MS. Thesis thesis, Universitas Airlangga.

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Abstract

The present study was to develop a specific and sensitive LC-MS/MS method for the determination of the low level of vitamin B12 (ng/mL) contained in solid multivitamin preparations. Liquid-liquid extraction was used for sample preparation, followed by liquid chromatography tandem spectrometric analysis and an electrospray-ionization interface. Vitamin B12 was separated from other components on the column of BEH C18 Waters (2.1 x 100 mm) with a particle size of 1.7 μm at a flow rate of 0.4 ml/minute and injection volume of 10μL. The chromatography condition was performed by using ammonium formate in water (2.5 mM): methanol with time program system. The analysis was conducted in positive-ESI mode by using multiple reaction monitoring (MRM). The method was validated in terms of specificity, linearity, precision, accuracy, LOD, LOQ and robustness. Aims method showed good separation and fragmentation according to m/z with parent ions at m/z 678.5 and daughter ion detected at m/z 147.10, 148.10 and 358.80. The linearity test in the range from 4.0 to 6.0 ppb with r value of 0.99521 and % Vx0 of 1.553. The precision showed % RSD at concentration of 80%, 100% and 120% was 1.288%, 2.886%, and 0.931%, respectively. The % recoveries were between 96.158% and 104.519% with LOD of 1.288 ng / mL or 3.687 μg/g and the LOQ was 4.291 ng/mL or 12.261 μg/g. The method was robust in the small changes of the composition of ammonium formate in the mobile phase and of concentration of ammonium formate. Application of the method in solid multivitamin dosage of capsule and powder preparation resulted 5.098 ng / mL (79.645%) and 5.279 ng/mL (81.829%) in capsule, 4.619 ng / mL (92.537%) and 4.631 ng / mL (92.555%) in powder.

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