Authors:Sachin Navale, Vinod Kuber, and Shrinivas Bhope
A densitometric HPTLC method has been established for simultaneous quantification of sennosides A and B and gallic acid in a laxative polyherbal pharmaceutical dosage form. Aluminum plates coated with silica gel 60 F254 as stationary phase were used with toluene-ethyl acetate-formic acid-methanol 8:8:4:5 (v/v) as mobile phase. Densitometric analysis was performed at 270 nm. Amounts of sennosides A and B and gallic acid were 10.48, 9.03, and 2.96% (w/w) respectively. The method was validated for specificity, linearity, precision, repeatability, and accuracy. Calibration plots were linear in the concentration range 114.0–427.5 ng per band for sennosides A and B and 100–375 ng per band for gallic acid. The correlation coefficients were 0.995, 0.998, and 0.997 for sennosides A and B and gallic acid, respectively. Relative standard deviation (RSD, [%]) for instrumental precision and repeatability of the method was 0.74, 0.49, 0.43 and 1.11, 1.08, 0.89 for sennosides A and B and gallic acid, respectively. Recovery was 96.28–97.22% for sennoside A, 98.06–100.84% for sennoside B, and 97.09–98.07% for gallic acid. The method is simple, precise, specific, accurate, and economical. It can be used for routine analysis of formulations containing Senna (Cassia angustifolia) and Haritaki (Terminalia chebula) extracts.
Sodium polystyrene sulfonate (SPS) powder is in use for over 50 years for the treatment of hyperkalemia. SPS powder is official in United States Pharmacopoeia, British Pharmacopoeia and European Pharmacopoeia. However, till date, no study has been published on the assessment of organic impurities for this drug. The organic impurities in bulk drug and finished product are associated with their safety, efficacy and stability. A simple, rapid, specific, precise and an accurate HPLC method has been developed for the estimation of toxic organic impurities like styrene, naphthalene, divinyl benzene (DVB) and ethylvinyl benzene (EVB) from SPS bulk drug and finished product. The developed method was validated for specificity, accuracy, precision, linearity, limit of detection (LOD), limit of quantitation (LOQ), solution stability, ruggedness and robustness. The influence of acid, alkali, oxidative stress, photolytic stress, thermal stress and humidity stress conditions on SPS bulk powder and finished product has been studied and reported. The proposed method can be successfully employed for the impurity testing of commercial batches of the bulk drug and finished products of both sodium salt and calcium salt of polystyrene sulfonate.
Authors:Nitin Shelke, Vinodkumar Kuber, Shrinivas Bhope, and Ramchandra Jadhav
A simple, precise, and rapid HPTLC method has been established for simultaneous analysis of E-guggulsterone, Z-guggulsterone, 11-keto-β-boswellic acid (11-KBA), and 3-acetyl-11-keto-β-boswellic acid (A-11-KBA) in an anti-arthritic formulation. The method involves densitometric evaluation of E and Z-guggulsterone, 11-KBA and A-11-KBA after their resolution on pre-coated silica gel 60F254 plates with n-hexane-chloroform-ethyl acetate-methanol 10:3:3:1 (ν/ν) as mobile phase. Detection was at 254 nm. Good resolution was achieved, with RF 0.61 ± 0.03, 0.68 ± 0.03, 0.28 ± 0.03, and 0.39 ± 0.03 for E and Z-guggulsterone 11-KBA, and A-11-KBA, respectively. The method was validated for specificity, linearity, precision, accuracy, and robustness. The method was linear in the range 10–90 ng per band for E and Z-guggulsterone and 50–450 ng per band for 11-KBA and A-11-KBA. Recovery at 80, 100, and 120% was 96.93 ± 0.27, 97.39 ± 0.22, 97.60 ± 0.61, and 97.19 ± 0.41% for E- and Z-guggulsterone, 11-KBA, and A-11-KBA, respectively. The method is simple, specific, precise, accurate, reproducible, and gives results comparable with those from an HPLC method.