Routine Quality Control Testing Research Articles

Development and validation of an HPTLC method for the simultaneous estimation of Clonazepam and Paroxetine hydrochloride using a DOE approach

The present study examines simultaneous multiple response optimization using Derringer's desirability function for the development of an HPTLC method to detect Clonazepam and Paroxetine hydrochloride in pharmaceutical dosage form. Central composite design (CCD) was used to optimize the chromatographic conditions for HPTLC. The independent variables used for the optimization were the n-butanol content in the mobile phase, the chamber saturation time and the distance travelled. HPTLC separation was performed on aluminium plates pre-coated with silica gel 60 F254 as the stationary phase using n-butanol:glacial acetic acid:water (9:2:0.5% v/v/v) as the mobile phase. Quantification was achieved based on a densitometric analysis of Clonazepam and Paroxetine hydrochloride over the concentration range of 40–240ng/band and 300–1800ng/band, respectively, at 288nm. The method yielded compact and well-resolved bands at Rf of 0.77±0.02 and 0.34±0.02 for Clonazepam and Paroxetine hydrochloride, respectively. The linear regression analysis for the calibration plots produced r2=0.9958 and r2=0.9989 for Clonazepam and Paroxetine hydrochloride, respectively. The precision, accuracy, robustness, specificity, limit of detection and limit of quantitation of the method were validated according to the ICH guidelines. The factors evaluated in the robustness test were determined to have an insignificant effect on the selected responses. The results indicate that the method is suitable for the routine quality control testing of marketed tablet formulations.

Absorbance Correction Method for Simultaneous Estimation of Nifedipine and Metoprolol Succinate in Their Synthetic Mixture Using From Spectrophotometry

A new simple, economical, precise and accurate method are described for the simultaneous determination of Nifedipine (NIF) and Metoprolol Succinate (MET) in combined tablet dosage form. The proposed method was applied for the determination of Nifedipine and Metoprolol Succinate in synthetic mixture, for determination of sampling wavelength, 10?g/ml of each of NIF and MET were scanned in 200-400 nm range and sampling wavelengths were 313nm for NIF and 275.40nm for MET are selected for development and validation of absorption correction method. For this method linearity observed in the range of 5-25?g/ml for NIF and 25-125?g/ml for MET, and in their pharmaceutical formulation with mean percentage recoveries 100.68 and 100.33, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

Simultaneous determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation using spectrophotometric technique (Simultaneous Equation Method)

A new spectrophotometric method was developed for simultaneous determination of compounds with interfering spectra in binary mixtures without previous separation, showing significant advantages over the conventional methods regarding minimal data manipulation and applicability. The proposed method was applied for the determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation, for determination of sampling wavelength, 10 ?g/ml of each of PRO and HCT were scanned in 200-400 nm range and sampling wavelengths were 289 nm for PRO and 270 nm for HCT are selected for development and validation of simultaneous equation method. For this method linearity observed in the range of 10-50 ?g/ml for PRP and 5-25 ?g/ml for HCT, and in their pharmaceutical formulation with mean percentage recoveries 100.13 0.86 and 100.07 0.58, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

Authenticity analysis of citrus essential oils by HPLC-UV-MS on oxygenated heterocyclic components

Citrus essential oils are widely applied in food industry as the backbone of citrus flavors. Unfortunately, due to relatively simple chemical composition and tremendous price differences among citrus species, adulteration has been plaguing the industry since its inception. Skilled blenders are capable of making blends that are almost indistinguishable from authentic oils through conventional gas chromatography analysis. A reversed-phase high performance liquid chromatography (HPLC) method was developed for compositional study of nonvolatile constituents in essential oils from major citrus species. The nonvolatile oxygenated heterocyclic components identified in citrus oils were proved to be more effective as markers in adulteration detection than the volatile components. Authors are hoping such an analysis procedure can be served as a routine quality control test for authenticity evaluation in citrus essential oils.

Simultaneous determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation using spectrophotometric technique (Simultaneous Equation Method)

A new spectrophotometric method was developed for simultaneous determination of compounds with interfering spectra in binary mixtures without previous separation, showing significant advantages over the conventional methods regarding minimal data manipulation and applicability. The proposed method was applied for the determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation, for determination of sampling wavelength, 10 μg/ml of each of PRO and HCT were scanned in 200–400 nm range and sampling wavelengths were 289 nm for PRO and 270 nm for HCT are selected for development and validation of simultaneous equation method. For this method linearity observed in the range of 10–50 μg/ml for PRP and 5–25 μg/ml for HCT, and in their pharmaceutical formulation with mean percentage recoveries 100.13± 0.86 and 100.07± 0.58, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

Absorption Correction Method for Simultaneous Estimation of Nifedipine and Metoprolol Succinate in Their Synthetic Mixture Using From Spectrophotometry

A new simple, economical, precise and accurate method are described for the simultaneous determination of Nifedipine (NIF) and Metoprolol Succinate (MET) in combined tablet dosage form. The proposed method was applied for the determination of Nifedipine and Metoprolol Succinate in synthetic mixture, for determination of sampling wavelength, 10μg/ml of each of NIF and MET were scanned in 200–400 nm range and sampling wavelengths were 313nm for NIF and 275.40nm for MET are selected for development and validation of absorption correction method. For this method linearity observed in the range of 5–25μg/ml for NIF and 25–125μg/ml for MET, and in their pharmaceutical formulation with mean percentage recoveries 100.68 and 100.33, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

Antibacterial, antitussive, antioxidant and toxicological evaluation of Joshanda Lozenges

Article history: Received on: 23/02/2015 Revised on: 22/03/2015 Accepted on: 16/05/2015 Available online: 27/07/2015 Joshanda, a Greco-urban formulation comprising seven herbs has been used since centuries for the treatment of cold, cough and associated allergic reactions. Conventionally, it is used in the form of an extemporaneously prepared decoction. However, in the current scenario, lozenges happen to be the dosage form of choice for antitussive drugs. In case of polyherbal drugs, the dosage form assumes a great importance in order to ensure that all the phyto-components exert their pharmacological effect to the maximum. Based on the popularity of lozenges, conventional decoction form of Joshanda was formulated in the form of lozenges. Lozenges were evaluated for routine quality control tests. The most remarkable feature of the formulation was that excellent compression, hardness, friability and disintegration properties could be achieved without the addition of any external binder. The prepared formulation was subjected to in vitro antioxidant activity, antibacterial activity against common respiratory tract pathogens, in vivo antitussive activity and acute toxicity studies using Albino Wistar mice. Accelerated stability studies were conducted as per ICH guidelines. The performance of lozenges was found to be satisfactory in all the tested aspects. Our study proposes the use of lozenges as a preferred dosage form of the conventionally used decoction of Joshanda.

Simultaneous Determination of Propranolol Hydrochloride and Hydrochlorothiazide in Tablets Formulation using Spectrophotometric Technique (First Derivative Method)

A new spectrophotometric method was developed for simultaneous determination of compounds with interfering spectra in binary mixtures without previous separation, showing significant advantages over the conventional methods regarding minimal data manipulation and applicability. The proposed method was applied for the determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation, for determination of sampling wavelength, 10 μg/ml of each of PRO and HCT were scanned in 200-400 nm range and sampling wavelengths were 289 nm for PRO and 270 nm for HCT are selected for development and validation of simultaneous equation method. For this method linearity observed in the range of 10-50 μg/ml for PRP and 5-25 μg/ml for HCT, and in their pharmaceutical formulation with mean percentage recoveries 100.13± 0.86 and 100.07± 0.58, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

Establishment of in vivo - in vitro Correlation: a Cogent Strategy in Product Development Process

Background: In vivo In vitro correlation (IVIVC) development and its validation is an extremely important phase of dosage form (new as well as generic) optimization. It is a liaison (preferentially linear) between a suitable pharmacokinetic parameter (peak plasma drug conc. i.e. Cmax, time for peak plasma drug conc. i.e. tmax and Area under the Curve i.e. AUC) and in vitro characteristics. Need: During optimization modifications in formulation composition, manufacturing method, required equipments or even in batch size. If these changes are made, in vivo bioavailability study in healthy human volunteers may be required to prove bioavailability of newly developed dosage form with the earlier one. These facts halt the marketing of new formulation with added cost. Thus, it would be enviable to develop in vitro test that corresponds to bioavailability data. Applications: Thus the main purpose of development of IVIVC is to replace in vivo bioavailability and to support bio waivers. As IVIVC comprises linkage between suitable in vivo pharmacokinetic parameter to in vitro characteristic pertaining to dissolution; it can also be used to set up dissolution specifications and/ or validation of methods of dissolution studies. It also assists as means of quality control for certain SUPAC (Scale Up and Post Approval Changes). Moreover there must be some in vitro means to assure batch to batch consistency during large scale manufacturing. After successful establishment of IVIVC; dissolution method used in such establishment is used as routine quality control test as a measure of physiological performance of drug product.

Two smart spectrophotometric methods for the simultaneous estimation of Simvastatin and Ezetimibe in combined dosage form

Two simple, accurate, precise, sensitive and economic spectrophotometric methods were developed for the simultaneous determination of Simvastatin and Ezetimibe in fixed dose combination products without prior separation. The first method depends on a new chemometrics-assisted ratio spectra derivative method using moving window polynomial least square fitting method (Savitzky-Golay filters). The second method is based on a simple modification for the ratio subtraction method. The suggested methods were validated according to USP guidelines and can be applied for routine quality control testing.

Compounds from multilayer plastic bags cause reproductive failures in artificial insemination.

High levels of reproductive failure were detected in some Spanish sow farms in the Spring of 2010. Regular returns to estrus and variable reductions in litter size were observed. The problem started suddenly and did not appear to be related to the quality of the ejaculates, disease, alterations of body condition or any other apparent reasons. Subsequent studies determined that the problem was the origin of the plastic bags used for semen storage. Chemical analysis of the suspicious bags identified unexpected compounds such as BADGE, a cyclic lactone and an unknown phthalate that leached into the semen at concentrations of 0.2 to 2.5 mg/L. Spermatozoa preserved in these bags passed all of the routine quality control tests, and no differences were observed between storage in the control and suspicious bags (p > 0.05). In vitro fecundation tests and endocrine profiler panel analysis (EPP) did not show any alterations, whereas the in vivo tests confirmed the described failure. This is the first described relationship between reproductive failure and toxic compounds released from plastic bags.

Evaluation of the bubble point test of a 0.22-μm membrane filter used for the sterilizing filtration of PET radiopharmaceuticals

We developed a bubble point test kit and investigated the bubble point test of a 0.22-μm membrane filter used for the sterilizing filtration of [(18)F]FDG, [(11)C]MET and [(11)C]PIB. The bubble point test of the Millex-GS vented filter was often difficult due to air leakage from the vented portion of this filter. Therefore, to close the vented portion of this filter simply and reliably, we investigated the use of various materials. The bubble point test of the Millex-GS vented filter was performed by closing the vented portion of this filter with various materials, such as vinyl tape, plastic paraffin film (parafilm), urethane elastomer adhesive mat and polyethylene foam cushion tape. Gradually, the plunger inside a syringe filled with air was pushed down to increase the pressure on the pressure gauge and the bubble point test kit. Simultaneously, the pressure when a continuous stream of air bubbles that appeared out of the 0.22-μm membrane filter was measured as the product-wetted bubble point value. Then, the plunger inside a syringe filled with 10mL of water was pushed down to wash the 0.22-μm membrane filter. As in the case in the above-mentioned method of measuring the product-wetted bubble point, the water-wetted bubble point value was measured. The use of the polyethylene foam cushion tape and a double clip could easily and reliably prevent air leakage from the vented portion of the Millex-GS vented filter. In the bubble point test of [(18)F]FDG, [(11)C]MET and [(11)C]PIB, the product-wetted bubble point values were 382.7±6.9kPa, 385.4±6.2kPa and 351.6±7.6kPa, respectively. The bubble point ratio was used to determine the minimum product-wetted bubble point value. All results of the product-wetted bubble point test were beyond the minimum product-wetted bubble point value (334.4kPa ([(18)F]FDG), 334.4kPa ([(11)C]MET) and 310.3kPa ([(11)C]PIB)). Then, the water-wetted bubble point values were 396.5±8.3kPa, 395.8±8.3kPa and 390.3±7.6kPa, respectively. All results of the water-wetted bubble point test were beyond the filter manufacturer's minimum bubble point specification (344.8kPa). The bubble point test technique using the bubble point test kit was practical for routine quality control tests of PET radiopharmaceuticals.

Validated TLC-densitometry method for determination of cetirizine dihydrochloride in tablet dosage form

A rapid, reproducible and accurate TLC method was developed for the determination of Cetirizine Dihydrochloride in tablet. The analytes were dissolved with ethanol 70% and chromatographed on silica Gel GF 254 TLC plate using chloroform : methanol : ethyl acetate in the ratio of 2 : 7 : 3 (v/v) as mobile phase. Quantitative analysis was done through densitometric measurement at wavelength 234 nm. Method was found linear over the concentration range of 400 – 1600 ng/spot with the correlation coefficient of 0.996. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 75.54 and 226.64 ng/spot. The relative standard deviation of this method was 0.86% whereas the means of the recovery data was 100.54 ± 0.11%. The proposed method has been applied to the determination of Cetirizine Dihydrochloride in commercial tablet formulations and the result were 96.97 ± 0.86 % for brand A and 100.57 ± 1.17 % for brand B. The developed method was successfully used for the assay of Cetirizine Dihydrochloride. This method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v3i1.17294 International Current Pharmaceutical Journal, December 2013, 3(1): 208-210

Facial visible spectrophotometric determination of metformin hydrochloride in glucosam tablets and industrial waste water: Application to content uniformity testing

Objectives: To determine simple, accurate and highly sensitive spectrophotometric method for determination metformin hydrochloride in pharmaceutical preparations and in industrial waste water sample. Materials and Method: The method is based on the oxidation of metformin by a known excess of sodium hypochlorite in alkaline medium. Results: Formation of a yellow-colored chromophore having maximum absorbance at 385nm. Molar absorptivity was found to be 2 × 10 4 L.mol -1 .cm -1 . Beer’s law is obeyed in the concentration range of 0.5-4 µg .ml -1 , relative standard deviation (RSD) is better than ±1.8 (n =10) .The limits of detection and quantitation are 0.083 and 0.25 µg .mL -1 , respectively. The method is applied successfully to determination of metformin pharmaceutical formulation (tablets).The common excipients do not interfere with the proposed method. A statistical comparison of these results with those of official method using t and F values at 95% confidence level shows good agreements and indicated no significant difference in the precision, and the present method has good validity. Conclusion: The proposed method can be used as a routine quality control and content uniformity tests for determination of metformin in pure form, tablet formulations and industrial waste water sample.

Simultaneous determination of chloramphenicol and hydrocortisone acetate in cream using TLC desitrometry method

A rapid and reproducible TLC method was developed for the determination of hydrocortisone acetate and chloramphenicol in cream. The analytes were dissolved with methanol and chromatographed on silica Gel GF 254 TLC plate using chloroform:ethyl acetate in the ratio of 1:1.5 (v/v) as mobile phase. Spots at Rf 0.29 and Rf 0.59 were recognized as chloramphenicol and hydrocortisone acetate, respectively. Quantitative analysis was done through densitometric measurement at wavelength 265 nm. Method was found linear over the concentration range of 300-900 ng/spot with the correlation coefficient of 0.999 and 0.998 for hydrocortisone acetate and chloramphenicol, respectively. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 23.84 and 71.51 ng/spot for hydrocortisone acetate, 21.06 and 63.18 ng/spot for chloramphenicol. The precision of this method was less than 2.8% whereas the means of the recovery data were 100.40± 0.579% for hydrocortisone acetate and 100.24±1.20% for chloramphenicol. The proposed method has been applied to the determination of hydrocortisone acetate and chloramphenicol in commercial cream formulations and the recovery of label claim were 99.23±0.66% (chloramphenicol) and 99.25±0.41% (hydrocortisone acetate) for brand A and 100.32±0.87% (chloramphenicol) and 100.53±0.78% (hydrocortisone acetate) for brand B. The developed method was successfully used for the assay of hydrocortisone acetate and chloramphenicol. The method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v2i1.12871 International Current Pharmaceutical Journal 2012, 2(1): 7-10

Survey of compliance with European acceptability criteria for HVL and AEC

Half value layer (HVL) was measured for 226 general radiographic X-ray tube assemblies at 80 kV and for 53 dental X-ray tube assemblies at 70 kV, and evaluated by the previous (1997) and the new draft of European acceptability criteria (2009) for HVL as adopted from the IEC collateral standards. Fourteen per cent of the tested general radiography X-ray tube assemblies were subject to readjustment by the new criteria. In routine quality control tests, receptor entrance dose was estimated for 54 AEC systems by using post-exposure mAs values, taking into account the measured tube output at different tube potentials, HVL and estimated scattering for 10, 15 and 21 cm PMMA phantom. Receptor dose (third quartile) varied from 6.4 μGy at 60 kV to 3.8 μGy at 125 kV. The results correspond well to the draft criteria for maximum receptor dose of 10 μGy and for the patient thickness compensation.

Implementation of acceptability criteria for dental radiology in Belgium

The implementation of routine quality control (QC) tests in dental radiology in Belgium has been neglected for many years. In 2008, the (Belgian) Federal Agency for Nuclear Control determined acceptability criteria for X-ray equipment used for dentomaxillofacial imaging. An overview of the development of the criteria, together with implementation and the first results of dental QC in Belgium, is discussed.

Application of wavelets to the evaluation of phantom images for mammography quality control

The main goal of this work was to develop a methodology for the computed analysis of American College of Radiology (ACR) mammographic phantom images, to be used in a quality control (QC) program of mammographic services. Discrete wavelet transform processing was applied to enhance the quality of images from the ACR mammographic phantom and to allow a lower dose for automatic evaluations of equipment performance in a QC program. Regions of interest (ROIs) containing phantom test objects (e.g., masses, fibers and specks) were focalized for appropriate wavelet processing, which highlighted the characteristics of structures present in each ROI. To minimize false-positive detection, each ROI in the image was submitted to pattern recognition tests, which identified structural details of the focalized test objects. Geometric and morphologic parameters of the processed test object images were used to quantify the final level of image quality. The final purpose of this work was to establish the main computational procedures for algorithms of quality evaluation of ACR phantom images. These procedures were implemented, and satisfactory agreement was obtained when the algorithm scores for image quality were compared with the results of assessments by three experienced radiologists. An exploratory study of a potential dose reduction was performed based on the radiologist scores and on the algorithm evaluation of images treated by wavelet processing. The results were comparable with both methods, although the algorithm had a tendency to provide a lower dose reduction than the evaluation by observers. Nevertheless, the objective and more precise criteria used by the algorithm to score image quality gave the computational result a higher degree of confidence. The developed algorithm demonstrates the potential use of the wavelet image processing approach for objectively evaluating the mammographic image quality level in routine QC tests. The implemented computational procedures could also enable the performance of advanced analyses to study potential dose reduction in a routine service.

Development and validation of TLC densitometry method for the determination of Gliclazide in tablet dosage form

Some tablet pharmaceutical preparations containing Gliclazide as sole active ingredient, are marked now in Indone-sia. The determination of the component of preparation both qualitatively and quantitatively is important to ensure quality of the product. This research is aimed to develop a TLC method to analyze gliclazide in its single component tablet formulation. Gliclazide were dissolved with chloroform. Gliclazide was chromatographed on silica Gel 60 F254 TLC plate using toluene: ethyl acetate in the ratio of 1:1 (v/v) as mobile phase. Gliclazide showed Rf value of 0.58 and was scanned at 234nm using Camag TLC Scanner 3. This method validation showed a good linearity with correlation coefficient (r) of 0.999 while the coefficient of variation of the regression function (Vx0) = 2.406%. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method was respectively 28.78 and 86.35 ng/spot respectively. The mean absolute recovery of Gliclazide from the simulation sample was 100.5% ± 0.113 and the method precision was less than 5.3% whereas the mean of the recovery data was 100.3%. The proposed method has been applied to the determination of Gliclazide in commercial tablet formulations and the recovery of label claim were100.494%±0.348 for brand A and 100.111%±1.257% for brand B. The developed method was successfully used for the assay of gliclazide. The method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v1i10.11852 International Current Pharmaceutical Journal 2012, 1(10): 332-335

A smart simple spectrophotometric method for simultaneous determination of binary mixtures

A new simple spectrophotometric method was developed for the simultaneous determination of drugs with interfering spectra in binary mixtures without previous separation. The new method is based on a simple modification for the ratio subtraction method. This modification enabled wider range of application. The proposed ratio difference method was applied for the determination of brimonidine and timolol in laboratory prepared mixtures with mean percentage recoveries 100.40±2.29 and 101.23±1.30 respectively, and in their pharmaceutical formulation with mean percentage recoveries 101.08±0.44 and 100.66±0.52 respectively. The suggested ratio difference method was validated according to USP guidelines and can be applied for routine quality control testing.