Naslov
HPLC-DAD-ESI-MS analysis of atorvastatin and related impurities in bulk drug and pharmaceutical dosage forms

Autori
Mornar, Ana ; Damić, Miranda ; Nigović, Biljana

Vrsta, podvrsta i kategorija rada
Sažeci sa skupova, sažetak, znanstveni

Izvornik
13th International meeting Recent Developments in Pharmaceutical Analysis, Abstract book / R. M. Faccino - Milano : Universita degli Studi di Milano, 2009, 105-105

Skup
13th International Meeting Recent Developments in Pharmaceutical Analysis

Mjesto i datum
Milano, Italija, 09.09.2009. - 12.09.2009

Vrsta sudjelovanja
Poster

Vrsta recenzije
Međunarodna recenzija

Ključne riječi
Atorvastatin; Related impurities; HPLC; Mass spectrometry; ESI ionization

Sažetak
Atorvastatin is HMG-CoA reductase inhibitor used in the treatment of primary hypercholesterolemia by reducing the levels of total and low-density level cholesterol, triglycerides and apolipoprotein B in plasma. Treatment with atorvastatin is very long, so high purity of drug substances and the knowledge of the impurity profile are important criterions in a manufacturing process. HPLC-DAD-ESI-MSn is a powerful technique that combines the separation capabilities of liquid chromatography with the structural elucidation capabilities of tandem mass spectrometry. All experiments were done using Agilent 1100 Series LC/MSD Trap system. A Symmery C18 (150 mm x 4.6mm, 3.5 μ m) analytical column (Waters) was used for the HPLC separation of atorvastatin and its impurities. The mobile phase consisted of 10 mM amonium formate and acetonitrile (55:45, eluent A) and of acetonitrile (eluent B). The gradient program was as follows: 0% B to 12% B (18 min), 12% B isocratic (28 min), 12% B to 30% B (45 min) and 30% B isocratic (50 min). The column temperature was kept at 45 °C. The optimum wavelength was set according to maximum absorption in the UV spectra (λ = 246 nm). The MS system was operated with electrospray ionization source in the positive ion mode. Nitrogen was used both as drying gas at a flow rate of 10.0 L/min and as nebulizing gas at a pressure of 35.0 psi. The nebulizer temperature was set at 350 °C, and a potential of 3500 V was used on the capillary. The ion mass spectra were recorded in the range m/z 100– 800 and helium was used as collision gas. Optimized method allows separation of atorvastatin and its impurities (desfluoro atorvastatin, diastereomer of atorvastatin, atorvastatin methyl ester and atorvastatin lactone). Furthermore, the structure of unknown impurities was proposed according to their fragmentation data generated by MSn. The validation was performed under optimized chromatographic conditions, using both UV and MS/MS detection approaches. The applicability of the method was verified on real samples of pharmaceutical tablets containing atorvastatin at 10 and 20 mg levels.

Izvorni jezik
Engleski

Znanstvena područja
Farmacija

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