Current Issue : January - March Volume : 2012 Issue Number : 1 Articles : 12 Articles
Cleaning validation is the process of assuring that cleaning procedures effectively remove the residue from manufacturing equipment/facilities below a predetermined level. This is necessary to assure the quality of future products using the equipment, to prevent cross-contamination, and as a World Health Organization Good Manufacturing Practices requirement. We have applied the Total Organic Carbon (TOC) analysis method to a number of pharmaceutical products. In this article we discuss the TOC method that we developed for measuring residual amikacin on surface of mixing vessel during manufacturing process. The method with correlation coefficient R² = 0.988 and method offers low detection capability (0.89 parts per million) and rapid sample analysis time. The accurate recovery values ranged from 99.25±1.47 with method precision less than 2%RSD**. We found that the TOC method is applicable for determining residual amikacin on pharmaceutical surfaces and will be useful for cleaning validation....
HPLC stability-indicating method has been developed for the simultaneous determination of Butamirate citrate and Benzoic acid in pharmaceutical dosage forms. Active compounds were separated on Zorbax SB-C8 column (250 mm Ã?â?? 4.6 mm, 5 Ã?µm Agilent) at an ambient temperature. Elution was performed with a mobile phase consisting of acetonitrile (solvent A) and a mixture of 10 gm of sodium lauryl sulphate and 5ml of 1 N sulphuric acid in 1000 ml distilled water (solvent B) at a ratio of 70:30 v/v and a flow-rate of 1.7 ml/min. Detection was performed with UV detector at 205 nm. Cough syrup preparation was subjected to long-term stability in order to demonstrate that storage conditions and degradants from both active compounds did not interfere with the quantification of Butamirate citrate and Benzoic acid. Typical validation characteristics such as linearity, range, precision, accuracy, and selectivity were evaluated for Butamirate citrate and Benzoic acid. Using the novel method, both Butamirate citrate and Benzoic acid were separated successfully. Validation studies demonstrated that the novel method possessed a linear UV response, good system precision and accuracy, high sensitivity and specificity for Butamirate citrate and Benzoic acid....
Tyrosine acts as precursor for the biosynthesis of melanin via L-dopa. The darkening of potato tuber during physical injury was due to the conversion of tyrosine to melanin. The present work reports the simultaneous determination of L-dopa and tyrosine present in the aqueous extract of potato tuber through differential pulse voltammetric (DPV) technique using gold modified pencil graphite electrode (GPGE). It was found that tyrosine and L-dopa could be catalytically oxidized with diffusion-controlled characteristics at this electrode, which could be applied for the estimation of L-dopa present in biological samples. Oxidation peak potentials observed for L-dopa and tyrosine were at 204 mV and 659 mV respectively. The similar oxidation peak potentials were observed for the aqueous extract of potato tuber. The results demonstrated that the GPGE exhibited high electro-catalytic activity, high sensitivity and possess good analytical performance towards the simultaneous determination of L-dopa and tyrosine from potato tuber extract....
In the present work a gold modified pencil graphite electrode (GPGE) was used for the determination of insulin present in the pharmaceutical sample. Cresol, an electroactive phenolic compound present in insulin pharmaceutical sample which interfere for the detection of insulin. In this paper, the removal of cresol from dialysis process, than obtained solution was freeze dried, followed by detection of insulin by electrophoresis and differential pulse voltammetric (DPV) studies were achieved. The proposed method was applied for the determination of insulin in pharmaceutical sample....
Capsaicin has been recognized as the major component and it makes upto 70% of the total capsaicinoids. Capsaicin is the major of the capsaicinoids which produce pungency in chillies. It is a stable and powerful alkaloid. Capsaicin content varies with the variety, climate, geographical location, maturity when harvested, and the methods for processing or preservation. The present study deals with the estimation of capsaicin in five different varieties of Capsicum annuum and to ascertain the varieties which contain the most appreciable amounts of capsaicin. Capsaicin was detected and quantified in all the varieties studied by HPLC. The amount of caspsaicin varied from 37.92% to 44.46% (per 10 g of extract)....
The aim of present study is to isolate and characterize bioactive compound from Roscoea procera rhizomes. Roscoea procera rhizomes were extracted with ethanol (95%). This extract was studied phytochemically and bioactive compound is isolated by using thin layer and column chromatography technique. Compound was subjected to spectroscopic analysis such as FT-IR and 1H-NMR. Rf values of extract and isolated bioactive compound was found 0.042, 0.084, 0.136, 0.473, 0.600, 0.663, 0.736 and 0.67 respectively. Chromatographically pure compound was isolated by this method. It can be indicated that, isolated compound was found to be steroid or steroidal-glycoside and it was confirmed by spectroscopic analysis. As far as our knowledge goes this bioactive compound is novel and not reported in Roscoea procera rhizomes yet, which can provides deeper insights into indigenous method of application and effectiveness of plant derivatives in treating different ailments....
Background: We have developed a new approach to map localized inclusions of gold nanoparticles in the Intralipid-1% liquid phantom. Our goal was to show that combined spectroscopic and angular snapshots of liquid phantoms and phantoms with inclusions allow obtaining information relevant for prostate cancer diagnostics and treatment.\r\nMethods: A combination of the point radiance spectroscopy and white light spectroscopy was used to measure angular resolved light distribution in 450-900 nm spectral range in Intralipid-1% liquid phantoms with and without localized inclusions of gold nanoparticles.\r\nResults: Characteristic spectro-angular snapshots of the liquid phantom alone and with the localized inclusion of gold nanoparticles were obtained. For liquid phantoms without inclusions, the snapshots demonstrate wavelength dependent light distribution inside the turbid medium, visualize the transparency window and provide a quantification of angular spread of different wavelengths of light. For liquid phantoms with gold inclusions, the approach allows to isolate the spectroscopic signatures of the inclusions from the background, identify locations of the inclusions in the angular domain and quantify the detection limits in terms of the contrast value attainable for the selected quantity of gold nanoparticles located at the specific depth in tissue. A detection of 3x1013 particles up to 25 mm deep in Intralipid-1% was demonstrated.\r\nConclusions: The encouraging results indicate a promising potential of radiance spectroscopy in prostate treatment and diagnostics with gold nanoparticles....
ââ?¬Å?Recallââ?¬Â, is a jeopardizing condition for the company but in a way it strives for the betterment of the society. ââ?¬Å?Recallââ?¬Â, a word that sends larger and deeper shudders to the companies need to be addressed on right of way. It can ruin companyââ?¬â?¢s financial and market assets that may wreak havoc on all facts. Recalls are an appropriate alternative method for removing or correcting marketed consumer products, their labelling, and/or promotional literature that violate the laws administered by the Food and Drug Administration (FDA). Recalls are conducted by FDA request or on the initiative of the manufacturer. To emphasize on this article we have discussed few steps taken by industry to minimise recalls and measures to undertake recalls. This article expresses how drug recall is vital in quality of product, cGMP and health aspects of consumers. Article shares a case study from Sanofi Pasteur on its H1N1 vaccine production batches....
An isocratic reversed phase high-performance liquid chromatographic (RP-HPLC) method has been developed for the simultaneous determination of captopril and diuretics (furosemide and hydrochlorothiazide) in API, dosage formulations and human serum. Chromatographic separation was achieved on Purospher Start C18 (250 mm x 4.6 mm, 5 Ã?µm) and Hypersil ODS C18 (150Ã?â??4.6mm, 5micron) columns using mobile phase, methanol: water (70:30 v/v) adjusted to pH 3.0 via phosphoric acid 85% having flow rate of 1.0 mL min-1 at ambient temperature with detector set at 225 nm. Calibration curves were linear over range of 5-25 Ã?µg mL-1 with a correlation coefficient Ã?± 0.999. LOD and LOQ were in the ranges of 0.4-2.3 Ã?µg mL-1. Intra and inter-run precision and accuracy results were 98.0 to 102%....
Protein A-Sepharose affinity chromatography is a very successful method for the purification of immunoglobulins for pharmaceutical use. However, the chromatography efficiency and lifetime of this method have to be always adjusted to specific chromatography conditions (biological source, buffers, flow rates, antibody properties, temperature, protein concentration, cleaning protocol, etc). This study sought to demonstrate improvements in the performance of an established affinity chromatography procedure employed to purify the CB.Hep-1 monoclonal antibody (mAb) used in the purification of the active pharmaceutical ingredient of a Hepatitis B vaccine. In conclusion, the relative poor mAb recovery observed in 150 mM PBS; pH 8.0/100 mM citric acid; pH 3.0 buffer system conditions was attributed to the inefficacy of the elution buffer to disrupt completely interactions between the matrix and mAb. In this regard, retention of the CB.Hep-1 mAb into the matrix was helped by the ligand coupled to the matrix and not by unspecific interactions. The 1.5M glycine-NaOH/3M NaCl; pH 9.0/200 mM glycine-HCl; pH 2.5 buffer system significantly improved the affinity chromatography recovery without affecting mAb purity, molecular homogeneity, ligand leakage and mouse DNA content in 100 purification cycles. Thus, application of 1.5M glycine-NaOH/3M NaCl; pH 9.0/200 mM glycine-HCl; pH 2.5 as buffer system allowed the reduction of the CB.Hep-1 mAb and Hepatitis B vaccine costs, respectively....
Three simple, reliable methods were developed for the simultaneous determination of a mixture of Ambroxol HCl (A) and Guaifenesin (G) in presence of the oxidative degradate (AD) of A and guaicol (GD), the impurity of G . The first method is an isocratic HPLC method, where separation of the four components A, AD, G and GD was achieved on C18 column using water: methanol (80: 20, v/v, containing 1% triethylamine, pH 2.9) with a flow rate of 1.5 ml/min and UV detection at 220nm. A linear relationship in the range of 5-80 �µg.ml-1 and 10-150 �µg.ml-1 was obtained for A and G, respectively. The second method was a TLC-spectrodensitometric method, where the drugs together with AD and GD were applied on silica gel 60F254 plates and a mobile phase consisted of chloroform: methanol: ethyl acetate: acetic acid (70: 8: 12:10, by volume) was used for separation. Densitometric evaluation of the separated zones was performed at 270 nm. The regression analysis for the calibration plots showed good correlation over the range 1-7 �µg/ band and 2-10 �µg/band for A and G, respectively. The third method was a multivariate spectrophotometric calibration method where principal component regression (PCR) and partial least squares (PLS) methods were used for the determination of the four components A, AD, G, and GD. The three methods were applied to pharmaceutical dosage forms containing either ambroxol alone (drops, capsules and tablets) or A together with G (syrup). Model update of multivariate calibration was used to determine A and G in syrup dosage form due to interfering additives. Results for the three methods were statistically compared with those obtained by applying reference reported methods for the drugs and showed that the proposed methods are accurate, precise, and can be easily applied....
Three sensitive , selective and precise stability indicating methods for simultaneous determination of Paracetamol and Diphenhydramine hydrochloride in their binary mixture and in presence of P-aminophenol; the potential impurity and degradation product of Paracetamol; were developed. In Method A, Paracetamol was determined in presence of Diphenhydramine Hydrochloride and P-aminophenol using the first derivative (1D) spectrophotometric method by measuring the peak amplitude at 264.5 nm where linear relationship was obtained in the range of 2-12 �µg mL-1 while Diphenhydramine Hydrochloride was determined in presence of Paracetamol and P-aminophenol using the first derivative of ratio spectra (1DD) method at 224 nm. Method B utilized chemometric techniques [Principal Component Regression (PCR) and Partial Least Squares(PLS)] which successfully applied to quantify both drugs and degradation product using the information included in the absorption spectra of appropriate solutions of the three compounds in the range of 220-340nm. Method C used HPTLC-densitometric method in which the aforementioned components were separated on silica gel plates using chloroform-ethyl acetate-ammonia solution (4:6:0.2, by volume) as a developing system. This was followed by quantitative densitometric measurement at 220 nm .Linear relationship were obtained in the concentration ranges of 0.4-1.6 �µg/band , 3-12 �µg /band and 0.4-1.6 �µg/band for Paracetamol, Diphenhydramine Hydrochloride and P-aminophenol respectively. The proposed methods have been successfully applied to the analysis of Paracetamol and Diphenhydramine Hydrochloride in their pharmaceutical formulation without interference from other dosage form additives and the results were statistically compared with official method....
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