Acceptance Criteria For Accuracy Research Articles

Utility of Spectroscopic Studies for Quantification of Cefditoren Pivoxil in Commercial Samples

The current study is devoted to suggest new simple spectrophotometric probes for the estimation and quantification of cefditoren pivoxil (CFP) either in authentic or in commercial samples. Three simple kinetic and derivatize sensitive spectrophotometric methods were established. Two kinetic techniques (method A) and (method B) were based on the estimation of CFP using the oxidation properties of alkaline potassium permanganate at ambient temperature and the relation between the reduction in the absorbance of KMnO4 and the added CFP were also investigated. The intensity of absorbance (A) of the colored MnO4- ions were recorded at wavelengths 610 and 525 NM for the two methods, respectively. Method C was based on derivatization of CFP with 1,2-naphthoquinone-4-sulphonate reagent in a basic solution (pH=11) to produce an orange red colored solution exhibited the highest absorption peak (λmax) at 411 nm. The proposed systems displayed linearity over the concentration ranges of 1.0-16.0, 1.0-10.0 and 0.5-7.0 and#181;g mL-1.The suggested systems were validated obeying analytical methodology guidelines and the acceptance criteria for accuracy, precision, linearity, selectivity, and robustness were met in all cases.

Utility of Spectroscopic Studies for Quantification of Cefditoren Pivoxil in Commercial Samples

The current study is devoted to suggest new simple spectrophotometric probes for the estimation and quantification of cefditoren pivoxil (CFP) either in authentic or in commercial samples. Three simple kinetic and derivatize sensitive spectrophotometric methods were established. Two kinetic techniques (method A) and (method B) were based on the estimation of CFP using the oxidation properties of alkaline potassium permanganate at ambient temperature and the relation between the reduction in the absorbance of KMnO4 and the added CFP were also investigated. The intensity of absorbance (A) of the colored MnO4- ions were recorded at wavelengths 610 and 525 NM for the two methods, respectively. Method C was based on derivatization of CFP with 1,2-naphthoquinone-4-sulphonate reagent in a basic solution (pH=11) to produce an orange red colored solution exhibited the highest absorption peak (λmax) at 411 nm. The proposed systems displayed linearity over the concentration ranges of 1.0-16.0, 1.0-10.0 and 0.5-7.0 and#181;g mL-1.The suggested systems were validated obeying analytical methodology guidelines and the acceptance criteria for accuracy, precision, linearity, selectivity, and robustness were met in all cases.

Improved UV Spectrophotometric Method for Precise, Efficient and Selective Determination of Dexamethasone in Pharmaceutical Dosage Forms

An improved UV spectrophotometric method has been developed and validated for precise, efficient and selective determination of dexamethasone in tablets and capsules. The quantitative analyses were carried out using ethanol/water (2:1 v/v) as background electrolyte and UV detection was carried out at 240 nm. The calibration curve was linear over a concentration range from 4.0 to 40.0 µg mL -1 . The average recovery was 97.60 ± 1.06% for tablets and 96.64 ± 0.87% for capsules. The limit of detection and limit of quantification were 0.63 and 1.90 µg mL -1 , respectively. The method was validated according to ICH guidelines and the acceptance criteria for accuracy, precision, linearity, specificity and system suitability were met. The results obtained with proposed method confirm improved performance over other methods found in the literature . DOI: http://dx.doi.org/10.17807/orbital.v7i1.630

Development and validation of a reversed-phase HPLC method for simultaneous analysis of butylhydroxyanisol, simvastatin and its impurities in tablet dosage forms

A simple, rapid, and sensitive RP-HPLC method using photodiode array detection was developed and validated for the simultaneous determination of butylhydroxyanisol and simvastatin with its impurities in tablet forms. Chromatographic separation was achieved on a Phenomenex Hypersil (250×4.6 mm, 5 μm) column using the mobile phase acetonitrile-sodium acetate (12 mM) buffered to 4.2 with glacial acetic acid. The flow rate was 1.7 mL/min, and the UV detection were made at 238 nm for simvastatin and its impurities and at 290 nm for butylhydroxyanisol. The system suitability solution used for peak impurity identification was generated in-situ without use of any impurity reference standard. The method was validated according to ICH Q2(R1) guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, robustness, LOD, and LOQ, were met in all cases. Moreover, the reproducibility results obtained by 22 Official Medicines Control Laboratories (OMCL) of European Directorate were satisfactory. The compounds selected for impurity validation were based on those found during long term and accelerate stability studies carried out on several formulation tablets from Moroccan and other markets. The described method was robust and successfully applied in quality control laboratories for routine analysis to determine the butylhydroxyanisol and simvastatin with its impurities content in tablet dosage forms.

RP-LC gradient elution method for simultaneous determination of thiocolchicoside, aceclofenac and related impurities in tablet formulation.

Objective:The aim of the present study is to develop a simple and precise HPLC method for simultaneous determination of thiocolchicoside, aceclofenac and related impurities in a tablet formulation and validate as per ICH guidelines. The aim of study extends to perform forced degradation study to trace the degradation pathways of potential degradant impurities.Materials and Methods:The separation was achieved on a 4.6 mm × 100 mm, 3 μm C18 column at 40°C with the mobile phase containing 0.1 M ammonium acetate buffer and methanol in a gradient mode at a flow rate of 1.0 mL min−1. The UV detection was carried out at 257 nm.Results:Acelofenac, thiocolchicoside and their related compounds were well separated from each other with good resolution and symmetry factor without interference of excipients. The method for assay was linear in the range of 10-200 μg mL−1 for aceclofenac and 0.4 to 8 μg mL−1 for thiocolchicoside.Conclusion:The method was validated according to ICH guidelines and the acceptance criteria for accuracy, precision, linearity, specificity, robustness, ruggedness and system suitability were met in all cases. The method was highly specific, as two related compounds of thiocolchicoside and nine related compounds of aceclofenac were well separated from each other. Stress study ensured the specificity of the method as the unknown degradation products formed during stress studies did not interfere with the determination of thiocolchicoside and aceclofenac, thus proving the stability indicating capacity of the method.

Validation for Clinical Use of, and Initial Clinical Experience with, a Novel Approach to Population-Based Carrier Screening using High-Throughput, Next-Generation DNA Sequencing

Traditional carrier screening assays are designed to look for only the most common mutations within a gene owing to cost considerations. Although this can yield high detection rates in specific populations for specific genes (such as cystic fibrosis in Caucasians), they are suboptimal for other ethnicities or for patients of mixed or unknown ethnic background. Next-generation DNA sequencing provides an opportunity to provide carrier screening using more comprehensive mutation panels that are limited primarily by information about the clinical impact of detected sequence changes. We describe a next-generation DNA sequencing-based assay capable of reliably screening patient samples in a timely and comprehensive manner. The analytic accuracy in a research setting has been documented. Here, we describe the additional studies performed to ensure the accuracy (analytic validity) and robustness of our assay for use in clinical practice and provide data from our experience offering this testing. Our clinical experience using this approach to screen 11,691 invitro fertilization patients has identified 449 mutant alleles: 447 in carriers and 2 in an affected individual. In total, we found 87 distinct mutations in 14 different genes. Approximately one quarter of the mutations found are not included in traditional, limited, mutation panels, including 16 known mutations unique to our panel, and novel truncating mutations in several genes.

Performance of blood glucose meters in compliance with current and future clinical ISO15197 accuracy criteria

Since 2003, blood glucose meters for patient self testing are approved in Europe based on the accuracy performance criteria as defined by the ISO15197 guideline. A new draft ISO guideline is currently under regulatory review, which suggests more strict accuracy acceptance criteria, and which may not be entirely fulfilled by currently commercialized blood glucose meter systems. In order to investigate the compliance of BG*Star and iBG*Star and several other blood glucose meters with the new draft ISO guideline, we performed a post-hoc analysis of data obtained from a recently performed ISO-conforming clinical accuracy performance study. This study was performed with 106 patients, clinically presenting with blood glucose levels distributed over the entire measurement range and in line with the glucose distribution requirements as demanded by the guideline. The YSI 2300 STAT Plus analyzer (glucose oxidase) served as reference method.While all tested meters had been in a high degree of compliance with the current ISO criteria, performance was lower when analyzed in accordance with the new acceptance criteria (95% of readings have to be within ±15 mg/dL for values <100 mg/dL, and within ±15% for values ≥100 mg/dL). The following meters met the new criteria: Accu-Chek Aviva (95.5%/98.6%), BG*Star (98.5%/97.3%), iBG*Star (98.5%/97.3%), FreeStyle Freedom Lite (95.5%/96.6%), and OneTouch Ultra2 (95.5%/96.5%). One meter failed with low blood glucose values (Contour: 90.9%/95.9%).In conclusion, BG*Star and iBG*Star and several other branded meters met the new draft ISO15197 acceptance criteria, when tested in accordance with the instructions for use and with the ISO accuracy testing protocol in a clinical setting.

Stability-Indicating Methods for the Determination of Candesartan Cilexetil in Bulk Drug and Pharmaceutical Formulations

Abstract Two stability-indicating methods were developed for the determination of candesartan cilexetil in the presence of its degradation products. The first method uses isocratic RP-HPLC with an Agilent C18 column. The mobile phase was phosphate buffer (pH = 2.8 ± 0.1)–acetonitrile (60 + 40, v/v). The flow rate was 2.0 mL/min, and the UV detection was at 254 nm. The second method depends on TLC-densitometric measurements of drug spots at 254 nm. The separation was carried out on silica gel 60 F254 plates using ethyl acetate–methanol–toluene– ammonia 33% (40 + 25 + 20 + 2, v/v/v/v) mobile phase. The methods were validated according to U.S. Pharmacopeia guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, robustness, LOD, LOQ, and system suitability were met in all cases. Linear ranges of the methods were 10.0–200.0 μg/mL and 1.0–9.0 μg/spot for HPLC and TLC, respectively. The proposed methods were successfully applied to the drug in bulk powder, in laboratory-prepared mixtures with its degradation products, and in commercially available tablets. The results were compared statistically at the 95% confidence level with each other. There were no significant differences between the mean recovery and precision of the two methods.

Development and Validation of a Reversed-Phase Ultra-Performance Liquid Chromatographic Method for the Simultaneous Determination of Six Drugs Used for Combined Hypertension Therapy

A simple, rapid, and reliable ultra-performance LC assay method has been developed for the simultaneous estimation of orally administered hypertension drugs (atenolol, hydrochlorothiazide, amlodipine besylate, indapamide, nifedipine, and lercanidipine hydrochloride), any of which may be administered with atenolol in combined hypertension therapy. Chromatography was carried out at 25 degrees C on a 2.1 x 50 mm id, 1.7 microm particle size Acquity BEH C18 column with the isocratic mobile phase 0.01 M, 4.0 pH aqueous phosphate buffer-acetonitrile (50 + 50, v/v) at a flow rate of 0.35 mL/min. All drugs were separated in less than 4 min with good resolution and minimal tailing, without interference by excipients. The method was validated according to International Conference on Harmonization guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, and system suitability were met in all cases. The column effluent was monitored at 230 nm. The detector response was linear in the range of 1-20 microg/mL of these drugs. LOD obtained was 0.04 microg/mL for atenolol, 0.02 microg/mL for hydrochlorothiazide, 0.03 microg/mL for amlodipine besylate, 0.03 microg/mL for indapamide, 0.02 microg.mL for nifedipine, and 0.01 microg/mL for lercanidipine hydrochloride. The suggested method has the advantage that all the drugs can be quantified alone or in combination with atenolol using a single mobile phase.

Stability Indicating Method Development for Simultaneous Estimation of Ezetimibe and Atorvastatin in Pharmaceutical Formulations by RP-HPLC

Simple, specific, economical and precise high performance liquid chromatographic method for the simultaneous determination of ezetimibe and Atorvastatin in API (active pharmaceutical ingredient) and formulation has been developed and validated. Chromatography was carried out at 30°C on a prepacked Zorbax SB C18 (5 mm, 250×4.6 mm) column with the 0.02 M Potassium dihydrogen phosphate: Acetonitrile: Methanol (10:40:50, v/v/v) was used as the mobile phase. The UV detection was carried at 236 nm. The results obtained showed good agreement with the declared contents. Ezetimibe and Atorvastatin separated in less than 10 min with good resolution and minimal tailing and without interference of excipients. The retention times of ezetimibe and Atorvastatin were 5.7 min and 9.1 min, respectively. The method was linear in the range of 5–50 μg/ml for Ezetimibe concentration with a correlation co-efficient 0.9992 and in the range 5–60 μg/ml for Atorvastatin concentrations having correlation co-efficient 0.9994 and the recovery was 99-102%. The method was validated according to ICH guidelines and the acceptance criteria for accuracy, precision, linearity, specificity and system suitability were met in all cases. The proposed method can be used for quantitative determination of Ezetimibe and Atorvastatin combination from API and formulations.

A simple and rapid high-performance liquid chromatographic method for the determination of bisoprolol fumarate and hydrochlorothiazide in a tablet dosage form

A simple and precise high performance liquid chromatographic method has been developed and validated for the simultaneous determination of bisoprolol fumarate (BF), and hydrochlorothiazide (HCTZ) in a tablet formulation. Chromatography was carried out at 25 °C on a 4.6 mm × 250 mm, 5 μm cyano column with the isocratic mobile phase of 0.1 M aqueous phosphate buffer, acetonitrile and tetrahydrofuran (85:10:5, v/v/v) at a flow rate of 1.0 ml/min. The UV detection was carried out at 225 nm. HCTZ and BF were separated in less than 10 min with good resolution and minimal tailing, without interference of excipients. The method was validated according to ICH guidelines and the acceptance criteria for accuracy, precision, linearity, specificity and system suitability were met in all cases. The method was linear in the range of 50–150 μg/ml for BF and 125–375 μg/ml for HCTZ.

Proficiency tests in the determination of activity of radionuclides in radiopharmaceutical products measured by nuclear medicine services in 8 years of comparison programmes in Brazil

Proficiency tests were applied to assess the performance of 74 nuclear medicine services in activity measurements of 131I, 123I, 99Tc m, 67Ga and 201Tl. These tests produced 913 data sets from comparison programmes promoted by the National Laboratory for Ionizing Radiation Metrology (LNMRI) from 1999 to 2006. The data were evaluated against acceptance criteria for accuracy and precision and assigned as Acceptable or Not acceptable accordingly. In addition, three other statistical parameters were used as complementary information for performance evaluation which related to normative requirements and to radionuclide calibrators. The results have shown a necessity to improve quality control procedures and unsatisfactory performances of radionuclide calibrators, which incorporate Geiger–Müller detectors.