Routine Quality Control Research Articles

Stability Indicating Assay of Empaglifozin and Metformin

The newly developed stability‐indicating RP-HPLC method is simple, robust and validated on the basis of ICH guidelines for the simultaneous determination of Empaglifozin and Metformin hydrochloride in the tablet. Retention times under the optimized condition were 2.104 and 4.0822min for Metformin and Empaglifozin respectively. This research article indicates best separation of Empaglifozin and Metformin from their degradation products. Separation was achieved on a Sunniest ECO C18, 250mm x 4.6mm, 5µm analytical column at wavelength of 225nm, using a mobile buffer (pH-1.8): acetonitrile (50:50) in an isocratic elution mode at a flow rate of 1.2ml/min, Injection volume: 10µl and run time 6mins. The %RSDs for the precision studies was less than 1.5% for both drugs. The %RSD was less than 1.5% in all the parameters of robustness. The forced degradation studies were carried by using 0.1N HCl, 0.1 N NaOH and % 3 H2O2 and there is only % 7.2 degradation in an acidic medium for emplaglifozin and 11.63% for Meformin where as there was nothing degradation in basic and oxidative method. The analyte peaks were clearly separated from the degradant peaks in forced degradation studies. So this method is a fast, sensitive, robust and efficient high performance liquid chromatographic method for the concurrent determination of Metformin and Empaglifozin in their combination, and thus this method can be effectively employed for routine quality control works.

Determination of Genotoxic Impurities in Nilotinib using LC-MS Method

A validated HPLC method was developed for the determination of Nilotinib (Nob) in pharmaceutical formulation. Isocratic elution at a flow rate of 1.0ml/min was employed on Zorbax SB C18 5µm × 4.6mm, 150mm, or similar is used for this chromatography analysis and the column temperature is maintained as ambient. Mobile phase was a mixture of 2.00ml of acetic acid in 2000ml of water as mobile phase A and Acetonitrile 100% as mobile phase B was used. Rate of flow is identified at 1.3ml/min. a 50.0µl sample was injected. The run time is 20 minutes to Sample, blank, system suitability, and sensitivity solution. For the diluted standard solution, it is 60 minutes. The retention time was 1.30minutes. The% R.S.D Nob is identified. The mean percentage recovery for Nob is found within the specification limit. Due to this reason this proposed LC-MS method is successfully adopted to routine quality control analysis in formulations.

Development and Validation of HPTLC and First Derivative Spectrophotometric Methods for Determination of Levetiracetam in Bulk and Tablet Dosage Form

A simple, sensitive high performance thin layer chromatographic (HPTLC) method and first order derivative spectrophotometric methods were developed for estimation of US FDA drug levetiracetam in bulk and its tablet dosage form. Chromatographic estimation was carried out on silica gel 60 F245 TLC plate as stationary phase and toluene: methanol: Ethyl acetate (4:4:2v/v/v) as mobile phase. Densitometric analysis was carried out at wavelength 218nm. The Rf values for Levetiracetam was found to be 0.47±0.03. Linearity was observed over range of 400-3200ng/spot for Levetiracetam (R2 0.998). The %recovery of Levetiracetam was found to be 99.25-100.7%. The LOD and LOQ were found to be 0.0917ng/ml and 0.278ng/ml respectively indicating sensitivity of the method. The first order derivative spectra were obtained at n=4, Δλ=3nm and determinations was made at 215 nm using methanol as solvent. Linearity was observed in the range of 80μg/ml - 280μg/ml with good regression values. Percent mean recovery of Levetiracetam was obtained as 101.5%. Both proposed methods were simple, fast, accurate, precise and reproducible and hence can be applied for routine quality control analysis of levetiracetam in bulk and its tablet dosage form.

Breaking the Mold: Towards Rapid and Cost-Effective Microbial Contamination Detection in Paints and Cosmetics Using ATP-Bioluminescence

Traditional culture-based methods, though a “gold standard” for bacterial detection in various industrial sectors, do often not fulfill today’s high requirements regarding rapidity, on-site applicability, and cost-efficiency both during operation and evaluation. Here, the feasibility of using an adenosine triphosphate (ATP)-based assay for determining microbial contaminations in paints and cosmetics was investigated and compared with standard plate count techniques and dipslides. Therefore, we initially determined the level of sensitivity and assessed the accuracy and concordance among the different methods via spiking tests using a mix of frequently abundant bacterial species to simulate microbial contamination. Bioluminescence intensity was linearly proportional to log colony counts over five orders of magnitude (R2 = 0.99), indicating a high level of sensitivity. Overall, the accuracy varied depending on the test specimen, most probably due to matrix-related quenching effects. Although the degree of conformity was consistently higher at target concentrations ≥ 105 CFU·mL−1, microbial contaminations were detectable down to 103 CFU·mL−1, thus meeting the high requirements of various industries. ATP-based results tended to be within an order of magnitude lower than the reference. However, bearing that in mind, the developed assay serves as a rapid, real-time alternative for routine quality control and hygiene monitoring.

Simultaneous HPLC determination of remdesivir and dexamethasone in the presence of metformin, sitagliptin, and glimepiride in a synthetic mixture and spiked human plasma

The COVID-19 pandemic has raised many questions regarding the control and therapy of type 2 diabetes and the higher risk of severe disease progression. One of the therapeutic regimens used in moderate and severe cases of COVID-19, endorsed by the World Health Organization, involves the administration of an antiviral medicinal product and a corticosteroid. The present study describes the development of a liquid chromatographic method for the simultaneous separation and quantification of Remdesivir and Dexamethasone in the presence of Metformin, Sitagliptin, and Glimepiride in a synthetic mixture. The developed method also allows determination of Remdesivir, Dexamethasone, and Glimepiride in spiked plasma samples, using Sitagliptin as internal standard. A mixture of acetonitrile and potassium dihydrogen phosphate buffer (pH 3) in a ratio of 45:55 v/v was used as а mobile phase on a C18 column. The recovery percentages from plasma ranged from 85.1 to 108.5%. The developed method can serve in routine quality control and clinical laboratory practice.

Comprehensive analysis of vitamin D3 impurities in oily drug products using supercritical fluid chromatography-mass spectrometry.

Vitamin D3, an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D3 and five non-esters including four that are isobaric to vitamin D3. Firstly, a screening study highlighted the Torus 1-AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions. Secondly, make-up solvent composition and MS settings were optimized to reach high sensitivity. For both the separation and MS response, the screening design of experiments proved useful. Lastly, a fast saponification and liquid-liquid extraction method was developed, enabling efficient sample cleanup and impurities recovery from the complex oily matrix. The SFC-MS method suitability was assessed in two validation studies. The first study employed the ICH Q2 guideline for impurity limit test to demonstrate method specificity and establish a limit of detection (LOD) and a limit of quantification (LOQ) at 0.2% and 0.5%, respectively, for ester impurities. The second study conducted a comprehensive quantitative assessment for three non-ester impurities using a total error approach, determining method validity through accuracy profiles. The validated method exhibited reliable performance across impurity concentrations from 0.1% to 2.0%, with estimated LODs ranging from 2 to 7ng/mL. This study further promotes SFC-MS as a valuable, versatile, and green tool for routine pharmaceutical QC.

Elemental Characterization of Ambient Particulate Matter for a Globally Distributed Monitoring Network: Methodology and Implications.

Global ground-level measurements of elements in ambient particulate matter (PM) can provide valuable information to understand the distribution of dust and trace elements, assess health impacts, and investigate emission sources. We use X-ray fluorescence spectroscopy to characterize the elemental composition of PM samples collected from 27 globally distributed sites in the Surface PARTiculate mAtter Network (SPARTAN) over 2019-2023. Consistent protocols are applied to collect all samples and analyze them at one central laboratory, which facilitates comparison across different sites. Multiple quality assurance measures are performed, including applying reference materials that resemble typical PM samples, acceptance testing, and routine quality control. Method detection limits and uncertainties are estimated. Concentrations of dust and trace element oxides (TEO) are determined from the elemental dataset. In addition to sites in arid regions, a moderately high mean dust concentration (6 μg/m3) in PM2.5 is also found in Dhaka (Bangladesh) along with a high average TEO level (6 μg/m3). High carcinogenic risk (>1 cancer case per 100000 adults) from airborne arsenic is observed in Dhaka (Bangladesh), Kanpur (India), and Hanoi (Vietnam). Industries of informal lead-acid battery and e-waste recycling as well as coal-fired brick kilns likely contribute to the elevated trace element concentrations found in Dhaka.

Utility of sustainable ratio derivative spectrophotometry for the concurrent assay of synergistic repurposed drugs for COVID-19 infections; Insilico pharmacokinetics proof

The cutting-edge combination of fluvoxamine (FVM) and ivermectin (IVM) has been presented as a proposed dosage form for the treatment of COVID-19 infections in early diagnosed patients. The main objective of this work is to develop simple, sensitive, and efficient methods for the synchronous quantification of FVM and IVM without any prior separation. Four green UV-methods were employed for the synchronous quantification, namely: Fourier functions convolution of absorption spectra, FFAS, Fourier functions convolution of derivative spectra of absorption curves, FFDS, Fourier function convolution of ratio spectra of absorption curves, FFRS and the dual-wavelength method, DWM. FFRS and DWM approaches can be able to reconcile the two components' significantly interfering spectrum presented in this commixture. Good linearity was checked in the range of 5–40, and 2.5–25 μg/mL for the FVM, and IVM, respectively. All approaches developed have been recommended in compliance with ICH principles. Furthermore, the approaches’ greenness was predestined by “National Environmental Method Index” (NEMI), “Analytical GREEnness metric (AGREE)”, the “Analytical Eco-Scale”, and the “Green Analytical Procedure Index” (GAPI). In addition, spider diagram was utilized for the assessment of the greenness index of the solvent used. Beside greenness, the sustainability of our methods was investigated using the HEXAGON tool. Continuing the constant pursuit of greenness, drug-drug interactions (DDIs) between FVM & IVM were predicted by insilico tools to ensure the safety of the suggested mixture as a preliminary step before invitro and in vivo studies. Because they were deemed sustainable, affordable, and successful, the suggested UV-methods may be used for routine quality control investigations of the indicated formulations FVM & IVM.

Trace level quantification of N-nitrosorasagiline in rasagiline tablets by LC-TQ-MS/MS

Parkinson's disease is a chronic, progressive neurological disease that currently affects about more than 10 million population worldwide. Rasagiline is a selective, irreversible monoamine oxidase type B inhibitor used as monotherapy in early Parkinson's disease. Rasagiline tablets have been recalled from market due to the presence of unacceptable levels of nitrosamine impurity. European Medical Agency has set up very stringent limit 100ng/day of N-nitrosorasagiline (NSRG) in drug product based on its mutagenicity. The analytical methods need to be sufficiently sensitive in order to adequately detect and quantify trace levels of NSRG. A highly sensitive LC-MS/MS method for determination of NSRG in rasagiline tablet formulation was developed by effectively separating on zorbax eclipse XDB C18 column using 0.1% formic acid in mixture of water and acetonitrile (35:65 v/v) in an isocratic mode at 0.5mL/min flow rate. The measurement of NSRG was performed using triple quadrupole mass detection accompanied by electrospray ionization in the multiple reaction monitoring mode. The validation of the method was comprehensive, demonstrating strong linearity across the concentration spectrum of 2 to 200ng/mL for NSRG. The obtained correlation coefficient exceeded 0.998, signifying a robust relationship. Recoveries spanning from 80.0% to 120.0% for NSRG were deemed satisfactory. The developed method was able to detect and quantitate NSRG at a concentration level of 1 to 2ng/mL respectively (1 to 2ppm with respect to 1mg/mL of rasagiline tablet sample concentration). The developed and validated method can be employed for routine quality control testing of rasagiline tablets.

Rapid, Simple and Low-Cost Analytical Method Development for Quantification of Eltrombopag Olamine in Tablet Dosage by UV Spectroscopy Method.

Eltrombopag Olamine is a drug used to treat thrombocytopenia, a disorder where blood platelet counts get lower and severe aplastic anemia. It serves as a thrombopoietin receptor agonist, which give rise to platelet production in the bone marrow. The objective of this study is to develop a simple, specific, accurate, precise and economical Ultraviolet spectroscopy method to estimate the amount of Eltrombopag Olamine in bulk and tablet dosage form. The developed method was performed using methanol for identification and physicochemical characterization of the drug. The validation parameters like linearity, precision, accuracy, robustness limits of detection and quantitation, and specificity were assessed as per ICH Q2 (R2). The maximum absorbance wavelength (λmax) of the drug was found at 247 nm in methanol. The linearity was found in the concentration range of 2-14 μg/ml with regression equation y = 0.0619x - 0.0123 and r² = 0.999. The standard addition method was used to determine the accuracy of the developed method. The result was found in the % recovery range of 98-99%. The precision was done on λmax with respect to the parameters such as repeatability, intraday, and interday. The method was found to be precise as the % RSD value was found to be <2%. The detection limit value (LOD) and quantitation limit value (LOQ) were 0.0524 μg/ml and 0.1588 μg/ml, respectively. The developed method is simple, economical, accurate and selective. The developed method was adaptable for the estimation of Eltrombopag Olamine analysis in pharmaceutical dosage form and routine quality control laboratory.

RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR QUANTITATIVE ESTIMATION OF TEMOZOLOMIDE AND (S) - PERILLYL ALCOHOL IN NANOPARTICULATE DOSAGE FORM

A quick reverse-phase high-performance liquid chromatography (RP-HPLC) approach for the quantitative measurement of temozolomide (TMZ) and (s) - perillyl alcohol [(S)-POH] in a nanoparticulate system was developed and validated in the current work. The RP-HPLC method for the simultaneous estimation of TMZ and (S)-POH was developed using Agilent (Infinity 1260) HPLC system and ZorbaxC18 (4.6 x 150 mm i.d., 5µ; Agilent) as stationary phase. The optimized mobile phase comprised of ACN: water: MeOH (42:12:46 V/V/V; 42:08:50 V/V/V and 20:30:50 V/V/V) pumped at a flow rate of 0.8 mL min-1, 0.8 mL min-1 and 1 mL min-1, respectively. Drug separation was accomplished in an isocratic mode, and a PDA detector operating at 210 nm was used to track elution. The procedure was validated in accordance with ICH-Q2R1 standards. The responses of TMZ and (S)- POH were found to be linear at 50-175 μg mL-1 (ACN: water: MeOH 42:12:46 V/V/V and 42:08:50 V/V/V) and 50-175 μg mL-1 (ACN: water: MeOH 20:30:50 V/V/V) respectively. The percent recovery was determined to be between 97% and 103%, demonstrating that the method’s accuracy was adequate. The precision study’s percent relative standard deviation (% RSD) was less than 2, indicating the accuracy of the suggested procedure. It was discovered that the established method for the quantitative determination of TMZ and (S)- POH in bulk and in hollow gold nanoparticles was accurate, precise, and specific. The developed technique can be applied to TMZ and (S)- POH routine testing and quality control in bulk and nanoparticulate systems.

Validation of sorghum quality control (QC) markers across African breeding lines.

Sorghum [Sorghum bicolor (L.) Moench] is a cereal crop of critical importance in the semi-arid tropics, particularly in Africa where it is second only to maize (Zea mays L.) by area of cultivation. The International Crops Research Institute for the Semi-Arid Tropics sorghum breeding program for Eastern and Southern Africa is the largest in the region and develops improved varieties for target agro-ecologies. Varietal purity and correct confirmation of new crosses are essential for the integrity and efficiency of a breeding program. We used 49 quality control (QC) kompetitive allele-specific PCR single nucleotide polymorphism (SNP) markers to genotype 716 breeding lines. Note that 46 SNPs were polymorphic with the top 10 most informative revealing polymorphism information content (PIC), minor allele frequency (MAF), and observed heterozygosity (Ho ) of 0.37, 0.43, and 0.02, respectively, and explaining 45% of genetic variance within the first two principal components (PC). Thirty-nine markers were highly informative across 16 Burkina Faso breeding lines, out of which the top 10 revealed average PIC, MAF, and Ho of 0.36, 0.39, and 0.05, respectively. Discriminant analysis of principal components done using top 30 markers separated the breeding lines into five major clusters, three of which were distinct. Six of the top 10 most informative markers successfully confirmed hybridization of crosses between genotypes IESV240, KARIMTAMA1, F6YQ212, and FRAMIDA. A set of 10, 20, and 30 most informative markers are recommended for routine QC applications. Future effort should focus on the deployment of these markers in breeding programs for enhanced genetic gain.

Comparison of In vitro Dissolution Tests of five brands of Diclofenac Sodium delayed release tablets in Moroccan market

This study aims to evaluate the similarity of in-vitro dissolution profiles, of commercially available generics of diclofenac sodium delayed-release tablets, of 25mg strength, with the innovator brand in Moroccan Market. Dissolution profiles for five brands were determined using the paddle method from the United States Pharmacopoeia. For the aptitude verification of the method, in our experimental conditions, linearity and accuracy tests were performed. The rate of dissolution was determined by Ultra-Violet Spectroscopy at 276nm. The assessment between the generics and the brand medicine was carried out under the similarity factor approach. We also presented an overview of the dissolution principles of tablet dosage form, and the pharmacopoeia dissolution test recommendations in our case. To compliance with US pharmacopoeia specifications, the rate of dissolution should be not more than 10% after 2hours in the acid stage, and not less than 75% at 45 minutes in the buffer stage. Furthermore, two dissolution profiles are considered similar when the f2 value is ≥50. According to routine quality control, evaluating the rate dissolution at the final point, all the generic medicines marketed in Morocco, meet the specification of the dissolution testing. However, using the comparison of dissolution profiles, only generic-2 is interchangeable with the innovator brand.

Sustainable and white HPLC method for simultaneous determination of amlodipine and atorvastatin in film-coated tablet

This study presents a collaboration between academia and the pharmaceutical industry with one goal, to implement the transformation of the conventional into sustainable HPLC methods and to use these methods in the routine quality control of medicines. Therefore, a sustainable, fast, and robust high-performance liquid chromatography (HPLC) method for the determination of amlodipine (AML) and atorvastatin (ATV) in film-coated tablets was developed. The chromatographic separation was performed on stable bond C8 column (150 × 4.6 mm, 5 μm), using a mixture of ethanol and 0.02 M sodium dihydrogen phosphate monohydrate, pH 3.0 (63:37%, v/v) as a mobile phase. The optimized conditions enabled the determination of AML and ATV within 5 min, providing satisfactory results for system suitability parameters. The method was validated in accordance with the ICH guideline in terms of specificity, linearity, accuracy, and precision (repeatability and intermediate precision). The robustness of the method was confirmed using the Plackett-Burman experimental design. The greenness features of the method were assessed using the Eco-scale index, the AMGS calculator, and the AGREE tool. The high value of the whiteness score (93.5) confirmed that the method meets the requirements for the three main pillars (analytical, ecological, and economical) for the sustainable method development. The method was applied for the determination of both analytes in pharmaceutical dosage form (film-coated tablets that contains 10 mg AML and 10 mg ATV).

In-lab synthesized turn-off fluorescence sensor for estimation of Gemigliptin and Rosuvastatin polypill appraised by Spider diagram, AGREE and whiteness metrics

Gemigliptin-Rosuvastatin single-pill combination is a promising therapeutic tool in the effective control of hyperglycemia and hypercholesterolemia. Organic sensors with high quantum yields have profoundly significant applications in the pharmaceutical industry, such as routine quality control of marketed formulations. Herein, the fluorescence sensor, 2-Morpholino-4,6-dimethyl nicotinonitrile 3, (λex; 226 nm, λem; 406 nm), was synthesized with a fluorescence quantum yield of 56.86% and fully characterized in our laboratory. This sensor showed high efficiency for the determination of Gemigliptin (GEM) and Rosuvastatin (RSV) traces through their stoichiometric interactions and simultaneously fractionated by selective solvation. The interaction between the stated analytes and sensor 3 was a quenching effect. Various experimental parameters and the turn-off mechanism were addressed. The adopted approach fulfilled the ICH validation criteria and showed linear satisfactory ranges, 0.2–2 and 0.1–1 μg/mL for GEM and RSV, respectively with nano-limits of detection less than 30 ng/mL for both analytes. The synthesized sensor has been successfully applied for GEM and RSV co-assessment in their synthetic polypill with excellent % recoveries of 98.83 ± 0.86 and 100.19 ± 0.64, respectively. No statistically significant difference between the results of the proposed and reported spectrophotometric methods in terms of the F- and t-tests. Ecological and whiteness appraisals of the proposed study were conducted via three novel approaches: the Greenness Index via Spider Diagram, the Analytical Greenness Metric, and the Red–Green–Blue 12 model. The aforementioned metrics proved the superiority of the adopted approach over the previously published one regarding eco-friendliness and sustainability. Our devised fluorimetric turn-off sensing method showed high sensitivity, selectivity, feasibility, and rapidity with minimal cost and environmental burden over other sophisticated techniques, making it reliable in quality control labs.

Predicting the Mechanical Behavior of Additively Manufactured Mechanical Metamaterials Using Point Cloud Representation Learning

Abstract Additive manufacturing (AM) has been widely adopted to produce mechanical metamaterials for load bearing, energy absorption, and other applications in various industries such as aerospace, automotive, and healthcare. However, geometric imperfections largely exist in AM. Since the mechanical behavior of metamaterials is primarily dependent on their geometries, it is critical to evaluate how process-induced geometric imperfections affect the mechanical behavior of fabricated metamaterials. Most of the existing approaches for AM quality control concentrate on the detection of defects and are limited in their ability to assess defect-altered mechanical behavior of finished builds. Some studies leverage destructive tests or numerical methods for mechanical behavior assessment, which are costly and time-consuming, and impractical for high-throughput routine quality control. In this paper, a new machine learning framework is developed to predict the mechanical behavior of fabricated metamaterials based on their as-built geometries (represented as high-resolution point clouds). Specifically, the point cloud is first converted into an image profile, which preserves detailed geometric patterns. then, a deep neural network is constructed to encode salient features of the image profile and associate them with the load-deflection curve of the fabricated metamaterial. The effectiveness of the developed framework is experimentally validated through a case study with auxetic mechanical metamaterial. This work has great potential to be extended for in-process prediction of AM builds’ mechanical behavior based on layer-wise point cloud scanning.

Channelized hotelling observer-based low-contrast detectability on the ACR CT accreditation phantom: Part II. Repeatability study.

Objective and quantitative evaluation for low-contrast detectability that correlates with human observer performance is lacking for routine CT quality control testing. Channelized Hotelling observer (CHO) is considered a strong candidate to fill the need but has long been deemed impractical to implement due to its requirement of a large number of repeated scans in order to provide accurate and precise estimates of index of detectability (d'). In our previous work, we optimized a CHO model observer on the American College of Radiology (ACR) CT accreditation phantom and achieved accurate measurement of d' with only 1-3 repeat scans. In this work, we aim to validate the repeatability of the proposed CHO-based low-contrast evaluation on four scanner models using the ACR CT accreditation phantom. The repeatability test was performed on four different scanners from two major CT manufacturers: Siemens Force and Alpha; Canon Prism and Prime SP. An ACR CT phantom was scanned 10 times, each time after repositioning of the phantom. For each repositioning, 3 repeated scans were acquired at 24, 12, and 6 mGy on all four scanner models. CHO was applied at the measured dose levels for different low-contrast object sizes (4-6mm). The CHO was also applied to images created using deep learning-based reconstructions on Canon Prism and to four different scan/reconstruction modes on the Siemens Alpha, a photon-counting-detector (PCD)-CT. The repeatability was evaluated by the probability that a measurement would fall within the±15% tolerance (P<15% ). With the CHO setting optimized for the ACR phantom and the use of 3 repeated scans and 9 non-overlapping slices per scan, the CHO measurement could provide high repeatability with P<15% of 98.8%-99.9% at 12 mGy with IR reconstruction on all four scanners. On scanner A, P<15% were 91.5%-99.9% at the three dose levels and for all three object sizes while the numbers were 93.6%-99.998% on scanner B. P<15% were 96.5%-97.2% for the two deep learning reconstructions and 97.0%-99.97% for the four scan/reconstruction modes on the PCD-CT. The CHO provided highly repeatable measurements with over 95% probability that a CHO measurement would lie within the±15% tolerance for most of the dose levels and object sizes on the ACR phantom. The repeatability was maintained when the CHO was applied to images created with a commercial deep learning-based reconstruction and various scan/reconstruction modes on a PCD-CT. This study demonstrates that practical implementation of CHO for routine quality control and performance evaluation is feasible.

Evaluation of the Impact of Refined Quality Control Management Model on the Qualified Rate of Disinfection and Sterilization of Surgical Instruments in the Sterilization Supply Center

Objective: To evaluate the application value of a refined quality control management model for a sterilization supply center. Methods: A retrospective analysis was conducted on the work situation of the sterilization supply center from January 2021 to January 2023. The work situation before January 31, 2022, was classified as the control group; a routine quality control management model was implemented, and the work situation after January 31, 2022, was classified as the observation group. The quality of medical device management and department satisfaction between the two groups were compared. Results: The timely recovery and supply rate, classification and cleaning pass rate, disinfection pass rate, packaging pass rate, sterilization pass rate, and department satisfaction score in the observation group were all higher than those of the control group (P &lt; 0.05). Conclusion: Implementing a refined quality control management model in the sterilization supply center can improve the quality management level of medical devices and department satisfaction and is worthy of promotion.

Chromatographic analysis of triple cough therapy; bromhexine, guaiafenesin and salbutamol and pharmaceutical impurity: in-silico toxicity profile of drug impurity

Bromhexine (BR), guaiafenesin (GUF) and salbutamol (SAL) are formulated as Ventocough syrup® (with and without sugar), labeled to contain propyl paraben and sodium benzoate as inactive ingredients. They are used to make coughing more productive and easier. A crucial element and a major issue in the pharmaceutical industry is the control of organic related impurities to obtain safe and effective treatment. Guaiacol (GUL) is reported to be GUF related impurity that was proved to be extremely toxic (toxic rating class 5), and its use should be banned. In this work, In-Silico study and ADMET estimation were conducted to predict GUL pharmacokinetic properties and its toxicity profile. Additionally, two chromatographic methods were conducted to analyze the studied components along with GUF impurity in the presence of the labeled dosage form excipients. The In-Silico study assured that GUL has oral rat acute toxicity and it is considered to be skin sensitizer. On the other hand, the developed TLC- densitometeric method depended on using a mobile phase mixture of hexane: methylene chloride: triethylamine (5.0:6.0:0.3, by volume) as a developing system. UV-Scanning was performed immediately at 275 nm for SAL, GUF and GUL, while scanning at 310 nm was used for scanning BR. Linearity was established in the ranges of 0.25–4.0, 0.25–4.0, 0.5–8.0 and 0.1–1.6 µg/band for BR, SAL, GUF and GUL, respectively. In the developed HPLC method, separation was performed on X-Bridge® C18 column (250 × 4.6 mm, 5 μm) using a solvent mixture of 0.05M disodium hydrogen phosphate pH 3 with aqueous phosphoric acid: methanol (containing 0.3%, v/v triethylamine) (40:60, v/v). Detection was done at 225 nm and separation was achieved within 10 min. Linearity was proved in the range of 2–50 µg/mL for the proposed drugs. Validation of the developed methods was done and all the calculated parameters were within the acceptable limits recommended by ICH guidelines. After that, methods were used to examine the potency of the selected marketed dosage forms and concentrations of all drugs were within the acceptable limits. Additionally, complete separation between the studied drugs and the additives were observed. The developed methods can be used during routine quality control analysis of the proposed drugs when the required issues concern on sensitivity, selectivity and analysis time.Graphical

ECO-FRIENDLY METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF FENOFIBRATE AND ATORVASTATIN IN MARKETED FORMULATION

This study focuses on the development and validation of an eco-friendly analytical method for the simultaneous estimation of Fenofibrate (FNF) and Atorvastatin (ATV) in a marketed formulation. The stability of both drugs was evaluated using a mixed hydrotropic solution of 2M Ammonium Acetate and 2M Sodium Citrate (1:1). This work focuses on the development and validation of an eco-friendly method for the simultaneous estimation of Fenofibrate and Atorvastatin in a marketed formulation. The stability of both drugs in a mixed hydrotropic solution was confirmed, and the method exhibited good linearity, recovery, and precision. The validated method was successfully applied to analyze a tablet formulation, demonstrating its applicability in routine quality control. The use of environmentally friendly practices in analytical methods contributes to sustainable pharmaceutical analysis. KEYWORDS: Eco-friendly method, Fenofibrate, Atorvastatin, Hydrotropic solution, Validation, Marketed formulation, Simultaneous estimation.