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Development and validation of an HPLC method for determination of atorvastatin and its impurities with DAD and MS detector

Atorvastatin is one of the most often used drugs for treatment of hypercholesterolemia, and the therapy is daily and longeterm. Therefore it is very important to control atorvastatin content in active pharmaceutical ingredient and in the pharmaceutical formulation, and to identify and quantify present impurities. For the analysis Agilent 1100 Series HPLC system was employed and Symmetry C18 column (Waters) 150 mm x 4.6 mm, 3.5 μm was used. A binary gradient method was developed. Spectrums were measured with DAD detector at λmax 246 nm. MS detector was operated with electrospray ionization source in the positive mode. The ion mass spectra were recorded in the range m/z 100 - 800. Method was validated according to ICH guidelines. For the linearity determination of atorvastatin DAD detector was used in the concentration range 100 – 1200 μg/mL. LC/DAD method proved to be precise (RSD<3.9%) and accurate (R=99.83-103.27%), but not sensitive enough. Therefore for the determination of impurities MS detector was employed with a much lower limit of quantification. Linearity was determined in the 0.05 – 10 μg/mL concentration range, and LOQ was 21.5-70.8 ng/mL. The use of MS detector also enabled structural characterization of present impurities.

atorvastatin; impurities; HPLC; DAD detector; MS detector

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