A rapid, sensitive, and accurate ultra-fast liquid chromatographic method is developed for the determination of related substances and degradants of Solifenacin Succinate, an active pharmaceutical ingredient used in the treatment of overactive bladder. Chromatographic separation of Solifenacin Succinate, its related substances, and degradants was achieved using a Shimpack XR-ODS-II column and mobile phase system containing 10 mM potassium dihydrogen orthophosphate in water. The pH of the buffer was adjusted to 7.0 using triethyl amine (mobile phase A). LC-grade acetonitrile was used as mobile phase B, employing a binary-gradient program at a flow rate 0.5 mL/min. The resolution between the critical pair of peaks (Impurity A and analyte) was found to be greater than 3.5. The limits of detection and quantification (LOQ) of Impurity A, Impurity B, and the analyte were 0.2 and 0.6 μg/mL, respectively for a 5-μL injection volume. The percentage recovery of impurities in the presence of sample matrix ranged from 95 to 104 w/w. The test solution and mobile phase was observed to be stable up to 24 h after the preparation. The validated method yielded good results of precision, linearity, accuracy, robustness, and ruggedness. The proposed method is found to be rapid, accurate, and suitable for the quantitative determination of related substances and degradants during quality control of Solifenacin Succinate active pharmaceutical ingredient.
simple, specific, linear, accurate and precise reverse phase chiral HPLC method was developed for the separation of efavirenz enantiomers
by using the Lux Amylose-2 column containing amylose tris(5-chloro-2-methyl phenyl carbamate) as a stationary phase. The mobile
phase consists of 0.1 % formic acid in water and acetonitrile (55:45, v/v). The flow rate was kept at 1.0 mL/min and the detection
wavelength used 252 nm and the column temperature was set at 25 ºC. The limit of detection was 0.01 mg/mL and the limit of quantification
was 0.04 mg/mL. The linearity calibration curve of (R)-enantiomer was shown well from the range of 0.04 mg/mL to 0.4 mg/mL. The
values of the correlation coefficient were 0.999 and 0.999 for (R)-enantiomer and (S)-efavirenz, respectively. The percentage recoveries of
(R)-enantiomer from efavirenz drug substance were ranged from 93.5% to 107.5%. The results demonstrated that developed RP-chiral
HPLC method was simple, precise, robust and applicable for the estimation of (R)-enantiomer in efavirenz API. This method was validated
in as per ICH Q2 (R1) and USP validation of compendial methods <1225>.
For separation of abacavir sulfate enantiomers, normal phase chiral methods were reported. Handling of normal phase solvents for high-performance liquid chromatography is very difficult in quality control laboratories and also no reversed phase-chiral high-performance liquid chromatography method for separation of abacavir sulfate enantiomer in drug substance has been reported. A new and accurate isocratic reversed phase-chiral high-performance liquid chromatography method was developed and validated for the separation of abacavir sulfate undesired enantiomer in abacavir. The separation achieved on amylose derivative chiral column, i.e. chiralpak AD-H containing amylose tris-3,5-dimethyl phenyl carbamate using 0.1% triethylamine in a mixture of water, methanol, and acetonitrile as a mobile phase. The correlation coefficient values were 0.998 and 0.997 for the undesired enantiomer and the desired enantiomer of abacavir sulfate, respectively. The limit of detection was 0.01% and the limit of quantification was 0.03%. The precision enantiomer at limit of quantification level was evaluated through six replicate injections and the relative standard deviation of the peak response achieved is 2.5. The percentage recoveries of undesired enantiomer from abacavir sulfate drug substance were from 96.7 to 118.0%. The drug substance was subjected to stress studies. It was found to not degrade significantly under acidic, hydrolysis, and oxidative stress conditions.
DOI: http://doi.org/10.1002/sscp.202000080
The cover picture shows the development, optimization and validation of Reversed phase chiral HPLC method for separation of abacavir sulfate enantiomers. Abacavir sulfate is used in the treatment of HIV infection. The proposed method provides an accurate tool for the quantitative estimation of enantiomers in quality control laboratories by creating an eco‐friendly environment.
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