Routine Quality Control Testing Research Articles

UV-Visible Spectrophotometric Method Development and Validation for the Estimation of Curcumin and Tetrahydrocurcumin

Background: Curcumin shows degradation in the solution of high pH. There is a need for development of a method which can estimate the drug release precisely and accurately. The UV spectroscopy due to its simplicity and specificity is the most popular for method development for the determination of drugs. Objective: The present study was aimed to develop the UV-Visible spectrophotometric method for the assessment of curcumin and tetrahydrocurcumin (THC) using a stable solvent system. Method: The solubility of curcumin and tetrahydrocurcumin was determined at various physiological pH levels. Non-ionic surfactant, tween 80 was used with selected media to avoid the degradation of drugs. The selected solvent system was further validated according to guidelines of the international conference on harmonization (ICH) and the analytical parameters like linearity, veracity, sensitivity and accuracy were studied. Results: The solvent systems Phosphate buffer of pH 6.8+2% tween 80 and Phosphate buffer of pH 6.8+1% tween 80 were found optimum for estimation of curcumin and THC respectively. All the validation parameters were found within the range for developed methods. Conclusion: The proposed method is very simple and can be used for routine quality control testing of curcumin and tetrahydrocurcumin.

From the use of exposure index in quality control testing to the use of exposure index for quality control of clinical images

AimThe exposure index (EI) is used in routine quality control (QC) tests performed in the radiographic equipment installed in our hospitals. This study aimed at investigating the factors affecting the calculation of EI in QC and clinical images, and the implementation of target EI (EIT) and deviation index (DI) in clinical practice. MethodsThe EI is 100 times the incident air kerma (IAK) in μGy on the image receptor, using the RQA-5 X-ray beam quality. Conformance to this relationship was investigated in QC images and clinical images acquired using anthropomorphic phantom body parts and different examination protocols, tube potential settings and radiation field sizes. Furthermore, a survey on EIT and DI data from clinical images was performed. ResultsThough automatic exposure control (AEC) systems have been adjusted for an IAK of 2.5 μGy, for most anthropomorphic phantom images the EIs were far from 250, depending on the manufacturer, the anatomy imaged, and the examination protocol. Regarding the survey results, DI calculation was feasible in only 38 % of the systems, since for the rest EIT values have not been set. However, the rationale based on which EIT have been selected is unclear. Some systems use only one while others many different EIT values. ConclusionBefore using EI for quality control of clinical images image all receptors and AEC systems should be properly calibrated. Then, the methodology of selecting appropriate EIT should be refined, since the EI calculation may vary, depending on the manufacturer, the anatomy imaged, and the examination protocol.

Suitability System of Microbiological Method for Nystatin Potency Determination in the Routine Analysis Using Agar Diffusion Method

Nystatin is a polyene macrolide antifungal active which is used for the treatment of candidiasis and obtained from some species of Streptomycesbacteria. The present work describes the statistical suitability analysis for regular monitoring of the agar diffusion bioassay in a simple, inexpensive and time-saving process before potency determination. A balanced (symmetrical) two-dose parallel line assay model was applied using the agar well diffusion method for quantification of Nystatin in raw material and finished medicinal dosage form. The routine inspection methodology yielded good results and included calculations by the linear parallel model and by means of regression analysis and verified using analysis of variance (ANOVA). The assay is based on the inhibitory effect of Nystatin upon a standard strain as described in the United States Pharmacopeia (USP). The results of the post validation regular assays were treated statistically by ANOVA and the deviations (expressed as average ± standard deviation) from both raw and column totals were 0.702 ± 0.476 and 0.865 ± 0.468, respectively. The mean value of the variance ratio for regression and parallelism squares were 534.349 ± 212.546 and 0.596 ± 0.345, respectively. The study of Nystatin's ongoing analysis showed that the microbiological assay design is satisfactory with respect to the limiting values for the determination of the potency. The established balanced parallel line assay is reasonably stable and suitable and can be used for the regular drug analysis in routine quality control testing and the quantitation of Nystatin in pharmaceutical dosage form and raw material. Doi: 10.28991/SciMedJ-2021-0304-2 Full Text: PDF

Application of Central Composite Design for screening and Optimization of HPTLC method for simultaneous quantitation of Aprepitant, Dexamethasone and Ondansetron in their synthetic mixtures

New HPTLC method was developed and optimized for estimation of Ondansetron (OND), Dexamethasone (DEX) and Aprepitant (APT) in laboratory prepared ternary mixtures by using Central composite design (CCD). The independent variables used for the optimization were the acetone content in mobile phase (%mL), distance of developing solvent (cm) and saturation time (min). HPTLC Separation was performed on Precoated silica gel F254 aluminum plate (10X10 cm, 100μm thickness) with a mobile phase consisting of chloroform: methanol: acetone: ethyl acetate: ammonia (9:4:2:5:0.2 % v/v/v/v). Quantification of OND, APT and DEX were achieved based on a Densitometric analysis over the concentration range of 200-1200 ng/band, 500-1000 ng/band and 1000-2000 ng/band, respectively, at 254nm. The method was yielded dense and well-resolved bands at Rf values of 0.54± 0.02, 0.79±0.02 and 0.23±0.01 for OND, APT and DEX, respectively. The linear regression analysis for the calibration plots produced r2= 0.9997, r2= 0.9998 and r2=0.9997 for OND, APT and DEX, respectively. The method was validated according to the ICH guidelines. The robustness test was determined that the selected factors have an insignificant effect on the responses. The results indicated that the method is suitable for the routine quality control testing of OND, APT and DEX in their bulk form.

An Effective Stability Indicating RP-HPLC Method for Simultaneous Estimation of Lamivudine and Raltegravir in Bulk and Their Tablet Dosage Form

Background: In the current study, asimple and specific stability indicating RP-HPLC method was developed and validated for the determination of Lamivudine and Raltegravir in bulk drug and it tablet dosage form using an UV-detector. Good separation was achieved by isocratic ally on a Zorbax SB-Phenyl (150 × 4.6 mm, 3.5 μ, 80 A°) column, using a mobile phase composition of buffer (0.1% v/v Phosporic acid in water): Acetonitrile (40:60 v/v) at a flow rate of 1.0 mL/min. The eluted analytes detected at 260 nm wavelength.
 Results: Lamivudine and Raltegravir were eluted at 3.1 and 5.4 min respectively with run time 7 min. Linearity in the method was measured in the concentration range of 30 – 70 μg/mL and 60 – 140 μg/mL for Lamivudine and Raltegravirrespectively. The percentage recoveries of Lamivudine and Raltegravirwere determined to be 100.30% and 100.53%, respectively. The validation of the developed method is carried as per USFDA and ICH guidelines, and the degradants were well resolved from Raltegravir and Lamivudine peaks. The developed RP-HPLC method was highly precise, specific, sensitive, and stability indicating.
 Conclusion: The results of the analysis prove that thedeveloped RP-HPLC method is simple, economical and widely acceptable, which can be used in routine quality control tests in the industry.

Quantitative determination of cyanoacetic acid content in teriflunomide drug substance by ion chromatography using conductivity detector

BackgroundThe current study focuses on the development and validation of an analytical method for quantifying cyanoacetic acid (CAA) in teriflunomide drug substance using a high-performance ion chromatography (IC) with cation suppressed conductivity detection (TFM). Water was used as the diluent for preparing the sample solution, which was injected into a standard chromatographic device with 250 mm, 4.0 mm ID, and 5.0 μm particle size Metrosep A Supp 5 Ion exchange column and a suppressed conductivity detector. At a flow rate of 0.6 mL min−1 and a temperature of 40 °C, the mobile phase was delivered in an isocratic mode.ResultsCAA and TFM had retention times of 12.78 and 15.82 min, respectively. CAA has a limit of detection (LOD) of 33 μg/g and a limit of quantification (LOQ) of 101 μg/g, respectively. For LOD and LOQ accuracy, the percentage RSD of CAA is 1.7 and 1.2, respectively. The average CAA recovery percentage was found to be between 98.6 and 100.1%. With a value of 0.9998, the calibration curve yielded an excellent linear correlation coefficient for CAA. According to the ICH guidelines, all verification parameters are within the range, indicating that the system is stable.ConclusionThe elution time and run time in the currently developed ion chromatography analytical method have been reduced, demonstrating that the method is cost-effective and generally accepted, as well as simple and functional, and can be used in routine quality control tests in the industry.

A cost-effective HPLC-DAD method for quality and stability assessment of antihypertensive herbal extracts in their recently co-formulated nutraceutical product

Hypertension is a chronic public health crisis that results in worldwide morbidity and mortality. The use of herbal extracts as natural alternative for health promotion, prevention and treatment of diseases in humans is gaining popularity over the years. Hibiscus sabdariffa and Olea europaea herbs have received historical attention for their high nutritious and therapeutic values. In the present work, a novel and economic high performance liquid chromatographic (HPLC) method coupled with diode array detection (DAD) was developed for quality control and stability assessment of their co-formulated antihypertensive nutraceutical product (NW Roselle® capsules). The most abundant markers contributing to the therapeutic activity, namely, Delphinidin 3-sambubioside (DEL) and Oleuropein (OLE) were quantified simultaneously. Chromatographic separation was attained using an Inertsil C18, 250 × 4.6 mm, 5.0 µm column and a mobile phase consisted of acetonitrile - phosphate buffer, pH 3.0 ± 0.1 in a ratio of 30:70, v/v, pumped at a flow rate of 1.0 mL/min in an isocratic elution mode. The use of DAD permits proper wavelength selection for sensitive and selective quantitation of the separated markers as well as chromatographic peak purity assessment. Satisfactory separation was achieved within short analysis time without any interference from the matrix co-extracted constituents. The proposed method was validated in accordance to the ICH guidelines. Moreover, evaluating the stability of NW Roselle® capsules was performed under accelerated storage conditions in addition to shelf-life estimation. The developed method represents an efficient and economic analytical approach for the routine quality control and stability testing of a new combination nutraceutical product, with the aim of improving consumer’s wellbeing by tracking identity, strength and therapeutic effect throughout the shelf life.

Stability indicating method development and validation for simultaneous estimation and quantification of Ertugliflozin and Metformin in bulk and tablet dosage form

BackgroundA simple, economical, sensitive, authentic, and faithful technique was used for the study of simultaneous evaluation of Ertugliflozin and Metformin in tablet dosage forms. The Chromatographic analysis was performed isocratically by using a Phenomenex C18 column (150 mm × 4.6 mm, 5 μm), and a mobile phase containing acetonitrile and 0.1% OPA buffer, with a proportion of 40: 60% v/v was passed throughout the column maintained at a temperature of 30 °C with a flow rate of 1 ml/min. Approximately, 10 μl of drug solution was injected and the analytes were eluted at 220.0 nm.ResultsThe elution times of Ertugliflozin and Metformin were 2.226 min and 2.955 min, respectively. The percentage RSD of Ertugliflozin and Metformin are 0.60 and 0.59, respectively. The percentage recoveries of Ertugliflozin and Metformin were determined to be 100.55% and 99.40%, respectively. LOD, LOQ values of Metformin and Ertugliflozin obtained were found to be 0.10, 0.2 μg/ml and 0.03, 0.09 μg/ml, respectively. Regression equation of Ertugliflozin was y = 11287x + 1191 and y = 46270x + 161.0 for Metformin. All verification parameters are within the range according to the ICH guidelines, and the degradation products are also within the limits, which show that the method is stable.ConclusionIn the currently developed RP-HPLC analytical method, the elution time and run time is reduced, which proves that the method is economical and widely acceptable, also simple and practical, which can be used in routine quality control tests in the industry.

Effect on quality assurance program and radiation dosimetry in ISO certified cancer hospital during the first COVID-19 wave

Background: Medical Physics department plays a pivotal role in developing and maintaining the quality services of radiation diagnosis and treatment in a cancer hospital. In this paper, the impact of the first COVID-19 wave on quality assurance (QA) program of medical physics department in an ISO-certified (9001-2015) hospital was quantified along with personnel dosimetry of radiation workers. Methods: The number of monthly, quarterly, and annual quality control (QC) procedures was analyzed, and QA program was prioritized in nuclear medicine and radiology department depending upon the hospital needs during the pandemic. The effect on personnel dosimetry during COVID period and annual dose was measured. Results: The QC procedures declined by 42% at radiological facilities (X-ray, mammography, gamma camera) of our hospital. It was noted that low frequency annual QC tests were less affected as compared to high frequency routine QC tests. During peak time of COVID-19 (23 March-30 June 2020) in Pakistan, the department worked with reduced manpower (50%) and reduced work hours (33%). The working hours gradually increased to 50% in June, 75% in August, and full restoration of manpower and workhours happened in September 2020. Radiation doses of all employees remained well within limit of 20 mSv per annum but the average dose of medical physics radiation worker increased during COVID. Conclusion: COVID-19 has adversely affected quality assurance program. Care must be taken for all radiation workers as some employees may become overdosed due to radiation workload.

Quantitation of Pregabalin by HPLC-UV Method using Ninhydrin Derivatization: Development and Validation

Introduction: A simple and reliable high performance liquid chromatographic method has been developed for the quantitative determination of pregabalin in bulk and dosage form. Pregabalin, a γ amino butyric acid analogue, has negligible sensitivity to UV or fluorescence detection. Hence, it has been derivatized by ninhydrin to form a chromophoric complex that could be quantified by UV detection. Materials and Methods: The concentration of ninhydrin was set to 5 mg/ml and a phosphate buffer solution (pH 7.4) was used as a solvent for the reaction. The resultant complex was separated by HPLC and detected by a UV detector at 569nm wavelength. Results: The developed method showed a linear response within 50 to 600 μg/mL of pregabalin. The method was accurate with mean recovery values within 100 ± 2%. The repeatability of the method was established by intra-day and inter-day precision study. Finally, a commercial pregabalin capsule was assayed by the developed HPLC method including ninhydrin derivatization. The result of the mean assay was found to be 100.37 ±2.94 %. Conclusion: This is the first time we are reporting pregabalin analysis using ninhydrin derivatization for HPLC analysis. Therefore, the developed method can be considered as a significant improvement in pregabalin quantitation and it can be easily applied for routine quality control tests of pregabalin.

β-galactosidase and Annexin V/PI Assays as QC Tests for Manufacturing cGMP-Grade Wharton Jelly Derived Mesenchymal Stem Cells

Background: According to the guidelines for cGMP, strictly regulated procedures and quality control (QC) tests are required. However, none of the regulations by authorities suggested have β galactosidase and Annexin V/PI assays as QC tests. In this study, we aimed to demonstrate the feasibility of Annexin V and β galactosidase assays as valid cGMP compliant QC tests. Methods: Wharton’s Jelly derived mesenchymal stem cells (WJ MSCs) were isolated, characterized and screened as valid QC tests. In this study, in addition to routine QC tests, β gal assays were performed to confirm telomerase activity and Annexin V methods were used to confirm cell viability assays. Results: It was concluded that one donor (WJ MSC 3) has higher telomerase activity and it has lowest β gal activity at the same time (p<0,001). Only one donor showed significant difference in annexin V viability tests, indicating the importance of using automatic devices and Annexin V to manual tests for cell viability analysis (Muse: 92,48 ± 0,487% Flow Cytometry: 90,76 ± 1,116% p<0,01). Conclusion: With these existing data, telomerase activity and senescence levels may correlate and affect MSC quality in cell based therapy. In order to determine the viability values by adding Annexin V based automated methods could give more guaranteed results. Key words: Good Manufacturing Practice, SA b galactosidase, cell senescence, telomerase activity, Annexin V, cell based medicinal products. DOI: 10.7176/JSTR/6-12-07

Stability-Indicating RP-HPLC Method for the Estimation of Process-Related Impurities and Degradation Products in Fesoterodine Fumarate by Using a Mass Spectrometric Compatible Mobile Phase.

The objective of the present work was to develop a sensitive, selective, accurate and precise stability-indicating HPLC method for quantification of degradation products and process-related impurities in fesoterodine fumarate extended-release tablets. The degradation profile was studied by conducting forced degradation studies and all the degradation products formed during degradation were separated. A chromatographic separation was achieved by using Waters Symmetry C18, 250 × 4.6mm, 5μm column, maintained at 30°C. Mobile phase A (0.05% trifluoroacetic acid in water) and mobile phase B (90% of 0.02% TFA in methanol and 10% of water) were used in gradient elution mode. A total of 75μL of each solution was injected and peak responses were quantified at 220nm. The method was found specific, precise, accurate, linear, rugged, robust and sensitive. During stability studies of fesoterodine fumarate extended-release tablets, one unknown impurity at relative retention time 1.37 was found increasing beyond the identification threshold. This impurity was isolated by using Preparative HPLC and structure was elucidated using mass and NMR spectroscopy. This method is a simple, inexpensive HPLC method that can be used as a routine quality control test for the estimation of impurities in fesoterodine fumarate extended-release tablets.

Radiosynthesis and quality control testing of the tau imaging positron emission tomography tracer [18 F]PM-PBB3 for clinical applications.

Recently, we produced 11 C-labeled 2-((1E,3E)-4-(6-(methylamino)pyridin-3-yl)buta-1,3-dienyl)benzo[d]thiazol-6-ol ([11 C]PBB3) as a clinically useful positron emission tomography (PET) tracer for in vivo imaging of tau pathologies in the human brain. To overcome the limitations (i.e., rapid in vivo metabolism and short half-life) of [11 C]PBB3, we further synthesized 18 F-labeled 1-fluoro-3-((2-((1E,3E)-4-(6-(methylamino)pyridine-3-yl)buta-1,3-dien-1-yl)benzo[d]thiazol-6-yl)oxy)propan-2-ol ([18 F]PM-PBB3). [18 F]PM-PBB3 is also a useful tau PET tracer for imaging tau pathologies. In this study, we developed a routine radiosynthesis and quality control testing of [18 F]PM-PBB3 for clinical applications. [18 F]PM-PBB3 was synthesized by direct 18 F-fluorination of the tosylated derivative, followed by removal of the protecting group. [18 F]PM-PBB3 was obtained with sufficient radioactivity (25 ± 6.0% of the nondecay-corrected radiochemical yield at the end of synthesis, EOS), radiochemical purity (98 ± 0.6%), and molar activity (350 ± 94 GBq/μmol at EOS; n = 53). Moreover, [18 F]PM-PBB3 consistently retained >95% of radiochemical purity for 60 min without undergoing photoisomerization using a new UV-cutoff light (yellow light) fixed in the hot cell to monitor the synthesis. All the results of the quality control testing for the [18 F]PM-PBB3 injection complied with our in-house quality control and quality assurance specifications. We have accomplished >200 production runs of [18 F]PM-PBB3 in our facility for various research purposes.

An Automated Method for Quality Control in MRI Systems: Methods and Considerations

Objective: The purpose of this study was to develop an automated method for performing quality control (QC) tests in magnetic resonance imaging (MRI) systems, investigate the effect of different definitions of QC parameters and its sensitivity with respect to variations in regions of interest (ROI) positioning, and validate the reliability of the automated method by comparison with results from manual evaluations. Materials and Methods: Magnetic Resonance imaging MRI used for acceptance and routine QC tests from five MRI systems were selected. All QC tests were performed using the American College of Radiology (ACR) MRI accreditation phantom. The only selection criterion was that in the same QC test, images from two identical sequential sequences should be available. The study was focused on four QC parameters: percent signal ghosting (PSG), percent image uniformity (PIU), signal-to-noise ratio (SNR), and SNR uniformity (SNRU), whose values are calculated using the mean signal and the standard deviation of ROIs defined within the phantom image or in the background. The variability of manual ROIs placement was emulated by the software using random variables that follow appropriate normal distributions. Results: Twenty-one paired sequences were employed. The automated test results for PIU were in good agreement with manual results. However, the PSG values were found to vary depending on the selection of ROIs with respect to the phantom. The values of SNR and SNRU also vary significantly, depending on the combination of the two out of the four standard rectangular ROIs. Furthermore, the methodology used for SNR and SNRU calculation also had significant effect on the results. Conclusions: The automated method standardizes the position of ROIs with respect to the ACR phantom image and allows for reproducible QC results.

Trade-off efficacy and data processing strategy in the power of spectral resolution of co-formulated antihypertensive pharmaceuticals.

Versatile, extraction-free univariate spectrophotometric methods have been modified to get effective spectral resolution of mixtures in accordance with their feature challenges. The proposed methods have been applied and validated for analyzing some antihypertensive medicines in their co-formulated medicinal products. Two mixtures have been used: the first one [Mix I (OLM/ADB)] is composed of Olmesartan medoxomil (OLM) and Amlodipine besylate (ADB) with partly-overlapped spectra while the second [Mix II (TEL/HCT)] is made up Telmisartan (TEL) and Hydrochlorothiazide (HCT) with total-overlapped spectra. Induced dual wavelength, absorbance correction and ratio subtraction coupled with constant multiplication methods were applied to Mix I (OLM/ADB), while dual wavelength, advanced absorbance subtraction and constant center coupled with spectrum subtraction methods were applied to Mix II (TEL/HCT). Calibration graphs were established with good correlation coefficients. The methods exhibit significant advantages as simplicity, sensitivity, minimal data manipulation besides optimum robustness. Selectivity was inspected using lab-mixtures with diverse ratios. Accuracy, precision and repeatability were found to be within the acceptable limits. The proposed methods are good enough to be used for co-assay of analytes in combined forms without any interfering from excipients. Moreover, all results were estimated in accordance with ICH criteria and successfully compared with those of the reported methods applying t-test and F-test at 95% confidence level. Generally, these methods can be used efficiently for routine quality control testing.

Rapid TLC with Densitometry for Evaluation of Naproxen Stability

The purpose of the work was to develop such chromatographic conditions that allowed to separate as many naproxen degradation products as possible. In order to follow this process, thin-layer chromatography (TLC) coupled with densitometry and spectrodensitometry was used. A forced degradation study was performed using an ethanolic solution of naproxen spotted on silica gel plates, existing in the form of an aqueous solution at various pH values, and as solution prepared in saline and in hydrogen peroxide. Degradative effect of UV light on naproxen was watched in the context of naproxen spotted on plates precoated with silica gel and exposed to UV light, and also for its solution treated with UV light. However, the solution of naproxen prepared in water at pH ≈ 2.60 undergoes the largest changes as the results of its exposure to UV light during 10 h. Stressed samples of naproxen were analyzed by using a new and well validated TLC procedure including toluene (TOL)—acetone (ACE)—chloroform (CHL) (2:5:12, v/v/v) as mobile phase A and glacial acetic acid (AcOH)—n-hexane (Hex)—acetone (ACE)-(0.10:10:10, v/v/v) as mobile phase B. As the newly developed TLC-densitometric method can effectively separate the substances about pharmaceutical significance from products of its degradation, which are formed as a result of stress studies, is considered to be a good alternative and important tool in routine quality control and stability testing of naproxen in pharmaceutical formulations. These results indicate that proposed TLC-densitometric method is cost-effective, rapid, specific, accurate, and precise. This TLC procedure is comparable to HPLC and UPLC method in terms of detection the number of degradation products of naproxen. In addition, it realizes the criterion of linearity. A major advantage and novelty of proposed method is its low cost and ability to analyze examined drug and all degradation products simultaneously, including those which can be observed under intensive UV radiation exposure of naproxen solution which are not described by previous HPTLC studies available in the literature.

Validation protocol for current good manufacturing practices production of [15O]water for hybrid PET/MR studies

Oxygen-15 (O; t½ = 122.4 s) has been used for nuclear imaging experiments since the beginning of the field. With the advent of simultaneous hybrid PET/MR technology, [O]water has seen a resurgence and remains the gold standard method for quantitative blood flow studies. The short half-life presents a nontrivial challenge to applying current good manufacturing practices production methods to maintain patient safety. A two-vial production method was devised to ensure adequate mixing of [O]water vapour into buffered isotonic saline. For production validation, six batches of [O]water were prepared: sterility, quality control testing and four patient doses. The final dose also underwent quality tested. Routine quality control testing included the following: radiochemical identity and purity, radionuclidic identity and purity, appearance, pH, pyrogenicity, and filter integrity. Sterility was retrospectively confirmed. For validation, breakthrough Pt concentration was also measured. Consistent yields of 10-12 GBq (270-325 mCi) were obtained 3 min after bombardment. Overall, 26 [O]water batches underwent quality control testing under this protocol and all met or exceeded release specifications for clinical use. The multiple batch protocol proved to be a safe and effective means for producing [O]water. Furthermore, this protocol could be readily adapted by any facility attempting to produce [O]water for clinical studies. Compared with previous attempts at our site, the protocol outlined here was more consistent and reliable, improved production workflow and led to more available radioactivity for participant injection and QC testing.

Comparative evaluation of dissolution profile of drug in its formulation by UV spectrophotometry

The aim of the research work was to develop a method for comparative evaluation of dissolution profile of two different brands of Teneligliptin hydrobromide hydrate drug in its formulations containing using UV Spectrophotometer. Simple, precise and accurate UV-spectrophotometric method was developed for Teneligliptin hydrobromide hydrate using optimized dissolution parameters like as 900mL of Phosphate buffer pH 6.8 as a dissolution medium and paddle (type II) apparatus at a stirring rate of 100 rpm. The drug release was evaluated by UV spectrophotometric method using 243.2nm as detection wavelength. Developed method obeyed Beer’s-Lambert’s law in the concentration range of 0.5-25 ?g/mL, with correlation coefficient value less than 1. The percent drug amount released estimated by proposed method was nearly 100%, found to be in good agreement with label claim of marketed tablet formulation. The proposed method were validated as per ICH guidelines with respect to accuracy, precision, LOD, LOQ and found to be within limits. The proposed method can be adopted for routine quality control test for estimation of drug in formulation. Also the statistical data analysis of percent drug release of brand 1 and 2 were compared with preexisting dissolution data of literature by using F-test and t-test. Keywords: Teneligliptin hydrobromide, Spectrophotometric method.

Utilization of UPLC-tandem mass spectrometry for quantitation of colouring matters in dietary formulation

A simple and sensitive ultra-performance liquid chromatography with Tandem Mass Spectrometric detection (UPLC-MS/MS) method was developed and validated for the simultaneous quantitation of two food colouring matters, Curcumin (CUR) and Riboflavin (RIB). Chromatographic separation was done on Hypersil gold 50×2.1 mm (1.9 μm) column, with gradient programing of mobile phase starting with aqueous 0.1% formic acid and increasing the percentage of 0.1% formic acid in acetonitrile. The utilization of multiple reaction monitoring (MRM) improved the selectivity of detection and decreased the matrix effect. The method was linear in the range of 5-500 ng/mL for CUR and RIB. Intra- and inter-day reproducibility were within the accepted criteria. The method was successfully applied for the determination the laboratory prepared mixtures of the two selected colouring matters. The use of mass spectrometry enhanced the selectivity and sensitivity of detection which allows the robust use of the method in routine quality control tests of the two colouring matters (CUR and RIB).

Application of biological variation and six sigma models to evaluate analytical quality of six HbA1c analyzers and design quality control strategy

Objective To apply biological variation and six Sigma models to evaluate analysis performance of 6 HbA1c analyzers and design the new quality control strategy. Method We collected data of imprecision and inaccuracy from routine internal quality control (June 2017–December 2017) and proficiency test of NGSP, respectively. The coefficient of variance (CV)% and bias% were plotted in the biological variation and six sigma models. The new quality control strategy was designed by the sigma value and OPSpecs. The quality improvement was guided by the QGI. Results The analytical performance of 6 HbA1c analyzers in our laboratory were good in the routine model, However, 50% (3/6) and 67% (4/6) of the HbA1c analyzers reached the acceptable level in the biological variation and six Sigma model, respectively. We also design personalized control strategy and promote quality improvement by combining the sigma value, OPSpecs, and QGI. Conclusions Biological variation model and six sigma model could visually display the performance of 6 HbA1c analyzers and personalized control strategy could be designed based on the sigma value, OPSpecs, and QGI.