Chromatographic and spectrophotometric methods were developed according to Quality by Design (QbD) approach as per ICH Q8(R2) guidelines for estimation of propafenone hydrochloride in tablet dosage form. QbD approach was carried out by varying various parameters and these variable parameters were designed into Ishikawa diagram. The critical parameters were determined by using principal component analysis as well as by observation. Estimated critical parameters in HPTLC method include solvent methanol, mode of detection absorbance, precoated aluminium backed TLC plate (10 cm 10 cm), wavelength: 250 nm, saturation time: 20 min, band length: 8 mm, solvent front: 70 mm, volume of mobile phase: 5 mL, type of chamber: 10 cm 10 cm, scanning time: 10 min, and mobile phase methanol : ethyl acetate : triethylamine (1.5 : 3.5 : 0.4 v/v/v). Estimated critical parameters in zero order spectrophotometric method were solvent methanol, sample preparation tablet, wavelength: 247.4 nm, slit width: 1.0, scan speed medium, and sampling interval: 0.2, and for first order derivative spectrophotometric method it was scaling factor: 5 and delta lambda 4. The above methods were validated according to ICH Q2(R1) guidelines. Proposed methods can be used for routine analysis of propafenone hydrochloride in tablet dosage form as they were found to be robust and specific.
& Two novel simple and rapid liquid-liquid and solid phase extraction methods have been developed for determination of olmesartan in human plasma using zidovudine as an internal standard. Liquid-liquid extraction from spiked human plasma samples was done using Dichloromethane: acetic acid (5.5: 0.5, v=v) solvent, while solid phase extraction was carried out on a DSC MCAX cartridge. For HPLC, the mobile phase consisted of water acetic acid pH 4.5 and methanol (25:75) at a flow rate of 0.5 mL Á min À1 in isocratic mode. The calibration curve was plotted with a concentration range 10 lgmL À1 to 60 lgmL À1 . Recovery studies were carried out by LLE and SPE procedures with average recoveries 69.27% and 72.87%, respectively. For HPTLC the developing phase consisting of ethyl acetate methanol and acetic acid (8.0:2.0:0.05 v= v=v) and detection was carried out on 269 nm. The calibration curve was plotted over the concentration range of 200 ng to 600 ng. The average recoveries were 90.12% and 79.64% by LLE and SPE, respectively. The proposed method was validated as per US-FDA guidance.
The use of metals in traditional medicine is very often seen as a matter of concern these days. Metals are processed through various steps like Shodhana, Marana, Amritikaran etc., to convert them into Bhasmas, which are then used as a medicine in Ayurveda for internal consumption. Bhasmas are unique Ayurvedic metallic preparations with herbal juices/fruits widely used for treatment of variety of chronic ailments. One of the extensively used routine Ayurvedic practice is Tamra (Copper) Bhasma. If it is not prepared properly or Shodhana procedure is not done properly, it acts as poison. To indicate its toxic potential, Ashtamahadoshas (eight major ill effects) have been quoted in classics and due emphasis have been given to its Shodhana procedure. In present study, Tamra Bhasma prepared by Rasamarit type under Kupistharasayana method was adopted. The observation was that Tamra Bhasma at dose TED i.e 5.5mg/kg showed non-toxic effect as indicated by its morphological, behavioral, biochemical, hematological and histopathological studies in wistar rats.
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