The objective of the present study was to separate and develop a chiral high-performance liquid chromatography (HPLC) and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) technique to estimate the (+) and (-) enantiomers of Albaconazole and validate the individual enantiomer of the drug. Albaconazole is used to treat anti-fungal diseases. The stationary phase was reverse phase Chiralpak IG-3 (250 × 4.6 mm, 5 μm) and (100 × 4.6 mm, 3 μm), whereas the isocratic mobile phase was ethanol and diethyl amine (100:0.1% v/v ratio HPLC) Acetonitrile and 10 mM ammonium bicarbonate (90:10 v/v ratio LC-MS/MS) and the flow rate was 1.0 and 0.5 ml/minute. The resolution of the (+) and (-) enantiomers were monitored using HPLC diode array detector (DAD) 240 signal and LC-electrospray ionization-MS/MS in positive transition at 432.0 m/z (M + H) for Albaconazole. The retention time of the (+) and (−) enantiomers of the drug was 6.952 and 9.955 minutes and 2.905 and 3.780 minutes by HPLC and LC-MS/MS. The major benefits of the LC-MS/MS are related to its improved selectivity, precision and accuracy and the lower variability in comparison to the HPLC-DAD. This study provided a rapid, sensitive and novel selective method to evaluate the (+) and (-) enantiomers in active pharmaceutical ingredients by HPLC and LC-MS/MS.
Key words: Albaconazole, (+) and (-) Enantiomers, HPLC, LC-ESI-MS/MS and Validation
|
