Robustness Study and Superior Method Development and Validation for Analytical Assay Method of Atropine Sulfate in Pharmaceutical Ophthalmic Solution

Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical method variation parameters are based on pH variability of buffer solution of mobile phase, organic ratio composition changes, stationary phase (column) manufacture, brand name and lot number variation;flow rate variation and temperature variation of chromatographic system. The analytical chemical method for assay of Atropine Sulfate conducted for robustness evaluation. The typical variation considered for mobile phase organic ratio change, change of pH, change of temperature, change of flow rate, change of column etc. Purpose: The aim of this study is to develop a cost effective, short run time and robust analytical chemical method for the assay quantification of Atropine in Pharmaceutical Ophthalmic Solution. This will help to make analytical decisions quickly for research and development scientists as well as will help with quality control product release for patient consumption. This analytical method will help to meet the market demand through quick quality control test of Atropine Ophthalmic Solution and it is very easy for maintaining (GDP) good documentation practices within the shortest period of time. Method: HPLC method has been selected for developing superior method to Compendial method. Both the compendial HPLC method and developed HPLC method was run into the same HPLC system to prove the superiority of developed method. Sensitivity, precision, reproducibility, accuracy parameters were considered for superiority of method. Mobile phase ratio change, pH of buffer solution, change of stationary phase temperature, change of flow rate and change of column were taken into consideration for robustness study of the developed method. Results: The limit of quantitation (LOQ) of developed method was much low than the compendial method. The % RSD for the six sample assay of developed method was 0.4% where the % RSD of the compendial method was 1.2%. The reproducibility between two analysts was 100.4% for developed method on the contrary the compendial method was 98.4%.

Development and Validation of a UPLC Method for the Determination of Docetaxel and Its Related Substances in Pharmaceutical Dosage Forms, an Antineoplastic Agent

A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.

Development, Translation and Validation of the Circle of Life (CoL) Satisfaction Scale Assessment Tool: An Integrative Nutrition Approach

Objectives: This study was designed to validate, test and translate a newly developed assessment tool for health coaches to assess client’s satisfaction rates of the Circle of Life (CoL), as a guide for weight management and also to monitor clients’ health and wellbeing improvements. This includes development of the assessment content, content validity, translating and pretesting the tool among potential clients. Method: 18 participants enrolled in a telenutrition weight loss program was and received a hypocaloric diet that was supported with monthly telemonitoring and health coaching sessions remotely for 6 months. Thus, we developed content of the assessment tool and created a rating scale of three levels of satisfaction (completely satisfied, slightly satisfied and not satisfied). The process of validation included content and language validity by experts in the field and language. Results: High scores according to the content validity rating were seen on both English and language versions of the CoL assessment tool by experts. Followed by a pre-testing process by participants, which showed reliability and consistency of the (CoL) variables using a multilevel analysis seeks across all individuals and all individuals had similar correlational pattern. Conclusions: The new (CoL) satisfaction scale have demonstrated a good capacity for identifying lifestyle factors associated with participants weight, which is a useful tool for integrative nutrition practice in weight management interventions. Future studies must be directed towards using the tool in assessing different populations and cultures to understand the main root of obesity in relation to behavior and day to day life factors.

Development and validation of an instrument to assess knowledge,attitudes,and practices on digital health among nursing officers

Objective:Validation is an important aspect of an instrument,and it ensures the confidence of researchers to employ the instrument in their studies.This study was conducted to develop and validate an instrument to assess knowledge,attitudes,and practices(KAP) on digital health among nurses since digital health capacity is a major concern in health care that needs to be assessed.Methods:We conducted a methodological study to assess the content validity and reliability of the instrument.First,items were generated through a comprehensive literature review and by obtaining an expert opinion.Second,content and face validity were assessed by a panel of 7 experts.Both the item-level content validity index(I-CVI) and the scale-level content validity index(S-CVI) were established.Moreover,test–retest reliability and internal consistency of the instrument were assessed.Data were analyzed using SPSS version 25.Results:The initial pool consisted of 60 items and after obtaining content,face,and construct validity,51 items remained.Items with an I-CVI <0.78 were considered relevant.The S-CVI for relevancy,clarity,ambiguity,and simplicity were 0.93,0.91,0.94,and 0.92,respectively.Five subcomponents were constructed in each knowledge and attitudes domain,and the test–retest reliability test revealed that the instrument has good reliability,showing correlation coefficient values for the KAP domains and the total questionnaire of 0.76,0.98,0.99,and 0.99,respectively.The independent Cronbach's α for all items was 0.76,indicating good internal consistency.Conclusions:The present study established the acceptable validity and ensured the good reliability and internal consistency of the instrument,which can serve as an assessment tool of KAP on digital health among healthcare professionals.

Quality Control of Tramadol in Kisangani: Development, Validation, and Application of a UV-Vis Spectroscopic Method

Context: Substandard and falsified medicines are circulating in low-income countries mostly without any control. We availed a simple and not expensive UV-Vis spectroscopic method to evaluate the quality of tramadol in Kisangani before and during the Covid-19 period. Methods: For the analytical quantitative method, an experimental design was applied to set up the optimal levels of the selected factors, namely, pH of dissolution medium, type of cuvette, and wavelength. Taking into account the capsule pharmaceutical formulation within 80 - 120 μg·mL-1 concentration range, we analyzed 89 tramadol samples from pharmacies and hospitals of the six Kisangani municipalities. Results: pH showed a significant effect on absorbance, whereas quartz cuvette and wavelength did not. A typical 100 μg·mL-1 tramadol solution gave an absorbance of 0.64 at 272 nm. Validation highlighted a matrix effect observed with a 6% bias. A correction factor of 0.9372 allowed to improve the accuracy profile, which were then totally included within the 10% acceptance limits. Quality control revealed that 25 samples out of 89 were not compliant in terms of manufacturing license, registration status in DRC and content as well. Conclusion: This study showed that the strengthening of analytical strategy in Kisangani is a need.

Development and validation of RP-HPLC method for determination of acetazolamide, furosemide and phenytoin extemporaneous suspensions

The development of the extemporaneous preparations allows physicians to adjust the dose for pediatric patients and provides for a more convenient dosage vehicle for those patients with difficulty swallowing tablets[1].As such,the production unit of pharmacy division,Sappasit Prasong Hospital,Ubon Ratchathani province,prepared the extemporaneous formulations such as Acetazolamide(AM),Furosemide(FM)and Phenytoin(PT)powder for suspensions.The extemporaneous suspensions of 10 mg/mL AM,2 mg/mL FM and 10 mg/mL PT were prepared from 250 mg Diamox?,40 mg Lasix?and 50 mg Dilantin?tablets,respectively and diluted with syrup vehicle.

A Stability Indicating Reverse Phase-HPLC Method Development and Validation for the Estimation of Rucaparib in Bulk and Pharmaceutical Dosage Form

The research was carried out for establishing a new reverse phase-HPLC stability indicating method for the quantification of Rucaparib. The experiment was determined on Waters HPLC instrument using 996 photo-diode array detector. The separation was done by using symmetry C-18 ODS (25 cm × 0.46 cm internal diameter) 5 μm analytical column containing mobile phase of Phosphate buffer (0.02 M) and methanol [65:35% v/v] adjusted pH to 4.8 by adding dilute ortho phosphoric acid. The method was run at 1 ml·min-1 at 286 nm detection. The drug was eluted at 5.484 min. After developing the method, it was assured for the intended use by validation which was done according to ICH Q2B guidelines. The analytical parameters checked were linearity, accuracy, repeatability, intermediate precision, limit of detection, limit of quantitation, ruggedness and robustness. It was observed that the response of the detector was linear in the range of 6 - 14 μg/ml with correlation coefficient of 0.999. The results of all the parameters were found to be within the acceptance criteria. The stability indicating assay method was established by using the samples generated by forced degradation process. The forced degradation was carried out by subjecting the drug to acid, alkali, thermal, oxidative and photolytic degradation and the results showed that the degradation products were successfully separated from the drug. Hence, this can be applied perfectly later for the analysis of quality of the rucaparib drug.

Analytical Method Development and Validation of Filgrastim by UV and RP-UFLC Methods

The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar drug, Filgrastim. Filgrastim or recombinant methionyl granulocyte colony stimulating factor (rGCSF) is a glycoprotein. It has a biological action essential for proliferation and differentiation of hematopoetic and progenitor cells. The UV and RP-UFLC work was carried on a Shimadzu UV1800 Spectrophotometer and Shimadzu Prominence LC-20AD UFLC systems, respectively. The λmax of filgrastim was found to be 215 nm. The correlation coefficient by UV spectroscopy was found to be 0.9994 for the concentration range of 1 to 3 μg/ml in double distilled water. The Reverse phase UFLC was done by using Phenomenex C4 (25 cm × 0.46 cm internal diameter) 15 μ, 300 A° analytical column. The optimized mobile phase for binary elution was Acetonitrile and double distilled water (80:20) with a flow rate of 1 ml/min. The retention time of drug was at 3.2 min. It was observed that the response of the detector was linear in the range of 5 - 15 μg/ml with correlation coefficient value of 0.999. After developing the methods, it was assured for the intended use by validation of the analytical parameters like linearity, accuracy, precision, limit of detection, limit of quantitation, ruggedness and robustness. The results of all the parameters for both the methods were found to be within the acceptance criteria as per the International Council for Harmonisation (ICH) guidelines.

Development and validation of an HPLC-UV method for analysis of methylphenidate hydrochloride and loxapine succinate in an activated carbon disposal system

Unused medications have the possibility of being abused, causing serious harm to individuals who were not prescribed the drug. The Food and Drug Administration(FDA) recommends the proper disposal of unused prescribed medications to maintain safety and prevent environmental hazards. However, many of the current disposal techniques do not properly address safety. A drug disposal pouch containing granular activated carbon offers a unique disposal method to deactivate residual or expired medication in a convenient, effective, and safe manner. A robust and validated method for methylphenidate hydrochloride and loxapine succinate was developed using high-performance liquid chromatography(HPLC) and the deactivation efficiency of the disposal system was tested. Methylphenidate hydrochloride was analyzed on a C18 analytical column(250 mm ?4.60 mm, 100?) using acetonitrile-water(0.05%(v/v) trifluoroacetic acid) as the mobile phase at a flow rate of1.0 mL/min with a run time of 15 min and retention time of 7.8 min. Loxapine succinate was separated on a C8100?(250 mm ? 4.6 mm, 5 mm) column maintained at 25 °C using a flow rate of 1.0 mL/min. The run time was 10 min and the retention time of the drug was around 4.6 min. Mobile phase was composed of acetonitrile and water(0.3% triethylamine) at pH 3.0 as 40:60(v/v). Reference standard solutions(100 mg/mL) for both drugs were prepared by dissolving in mobile phases. These methods provide good linearity(R2? 0.999) over the range of 5–100 mg/mL for methylphenidate hydrochloride and 0.1–100 mg/mL for loxapine succinate. The assay methods were successfully applied to study the deactivation of these drugs.

Analytical Method Development and Validation of Some Biosimilar Drugs by High Performance Thin Layer Chromatography

A simple and rapid HPTLC analytical method has been developed and validated for the determination of Etanercept and Filgrastim in pure form and in marketed formulation. Both the drugs were chromatographed on silica gel 60 F254s HPTLC plates, as stationary phase. The mobile phase optimized for Filgrastim and Etanercept was Water: n-butanol (7.5:2.5 v/v) and Isopropyl alcohol: water (6.5:4.5 v/v), respectively. The chromatogram obtained was scanned at 225 nm and 222 nm for filgrastim and etanercept which resulted in a retention factor of 0.45 ± 0.07 and 0.32 ± 0.03, respectively. The method was validated for parameters like linearity, accuracy, precision, specificity and robustness. Recovery studies were performed at three concentration levels, to demonstrate suitability, accuracy and precision of proposed method. Statistical analysis proved that the proposed method is accurate and reproducible with linearity in the range of 500 to 3000 ng/band for filgrastim and 200 to 1200 ng/band for etanercept. The limit of detection and limit of quantification for filgrastim was found to be 63.418 ng/band and 192.177 ng/band. For etanercept, LOD and LOQ were found to be 33.381 ng/band and 101.153 ng/band, respectively. The proposed method can be employed for the routine analysis of selected biosimilars.

A Stability Indicating Reverse Phase-HPLC Method Development and Validation for the Estimation of Bimatoprost 0.3% &Timolol 0.5% Pharmaceutical Ophthalmic Dosage Form

The research was carried out to establish a new reverse phase-HPLC stability indicating method for quantifying Bimatoprost & Timolol in ophthalmic solution. The experiment of Bimatoprost & Timolol in ophthalmic solution method development was determined on Waters HPLC instrument using a UV Detector. The separation was done by using L11, Zorbex SB phenyl (4.6 mm × 250 mm internal diameter) 5 μm analytical column, containing mobile phase of Phosphate buffer (0.02 M), methanol, and acetonitrile [50:30:20 % v/v]. The method was run at 1 ml·min-1 at 210 nm for Bimatoprost and 295 nm for Timolol for detection. The drug was eluted at 10.81 min for Bimatoprost and 3.77 min for Timolol. After developing the method, it was assured for the intended use by validation, which was done according to ICH Q2B guidelines. The analytical parameters checked were Specificity/Selectivity, linearity, Range, accuracy, ruggedness, and robustness. It was observed that the response of the detector was linear in the range of 6 - 18 μg/ml with a correlation coefficient of 0.999. The results of all the parameters were found to be within the acceptance criteria. The stability-indicating assay method was established by using the samples generated by the forced degradation process. The forced degradation was carried out by subjecting the drug to acid, alkali, thermal, oxidative, and photolytic degradation, and the results showed that the degradation products were successfully separated from the drug. Hence, this can be applied perfectly later for the quantitative analysis of Bimatoprost 0.3% + Timolol 0.5% Ophthalmic Solution drugs for pharmaceutical use. Currently, there is no official method for Bimatoprost & Timolol combination products in USP or BP. Available research work related to single Bimatoprost or Timolol products was not suitable for testing Bimatoprost and Timolol combination drugs. Additionally, there is no stability-indicating method to test Bimatoprost & Timolol combination products which insist us to do research and develop a new reverse phase-HPLC indicating method which will be faster and more accurate.

Development and Validation of Stability Indicating RP-HPLC-PDA Method for Tenatoprazole and Its Application for Formulation Analysis and Dissolution Study

In the present study, comprehensive stress testing of tenatoprazole was carried out according to ICH guide-line Q1A (R2). Tenatoprazole was subjected to stress conditions of hydrolysis, oxidation, photolysis and neutral decomposition. Extensive degradation was found to occur in acidic, neutral and oxidative conditions. Mild degradation was observed in basic conditions. The drug is relatively stable in the solid-state. Successful separation of drug from degradation products formed under stress conditions was achieved on a Kromasil C18 column (250 mm × 4.6 mm, 5.0 μ particle size) using methanol: THF: acetate buffer (68:12:20 v/v) pH adjusted to 6.0 with acetic acid as mobile phase, flow rate was 1.0 mL●min–1 and column was maintained at 45°C. Quantification and linearity was achieved at 307 nm over the concentration range of 0.5 - 160 μg●mL–1 for tenatoprazole. The method was validated for specificity, linearity, accuracy, precision, LOD, LOQ and robustness.

Development and Validation of Stability Indicating LC Method for 10-Hydroxycamptothecin

The present method gives a detailed description for the development and validation of a simple stability indicating reverse phase liquid chromatographic method for 10-hydroxycamptothecin(10-HCTN) in the presence of its impurities namely Imp A and Imp B along with degradation products generated from forced degradation studies. The drug was subjected to stress conditions of hydrolysis (acid, base and neutral), oxidative, photolytic and thermal stress degradation. Degradation was observed when subjected to treatment with peroxides or under conditions normally used for typical acid and base hydrolysis. The drug was found to be stable under other stress conditions attempted such as photolytic and thermal. Successful separation and isolation of the drug from related impurities and degradation products formed under stress conditions was achieved on an Inertsil ODS-3V (250 mm × 4.6 mm, 5 μm) column using a phosphate buffer, acetonitrile, methanol and Nanopure water. The developed HPLC method was validated with respect to specificity, linearity, accuracy, precision, sensitivity, robustness and solution stability. The assay method was found to be linear in the range of 0.16 mg/mL to 0.24 mg/mL with a correlation coefficient of 0.999 and the linearity of the impurities was established from 0.02% (LOQ) to 0.3%. Recoveries of assay and impurities were found between 99.4% and 100.3%. The developed HPLC method can be used to determine the related substances and assay determinations of 10-HCTN and also to evaluate the quality and long term stability of production samples.

Development, Validation and Application of a Spectrofluorimetric Method for the Quantification of Nevirapine in Pharmaceutical Formulations Tablets and Suspensions

The development of the spectrofluorimetric method can be considered a promising alternative that is relatively less expensive and sufficiently reliable. In the current literature, no method for the analysis of nevirapine by spectro-fluorimetric has been reported. The proposed method is based on the transformation of naturally non-fluorescent nevirapine into a fluorescent derivative after chemical synthesis. Maximum excitation and emission wavelengths are 290 nm and 357 nm respectively. The analytical performance of the method demonstrates linearity in the concentration range 1.5 × 10-2 and 13.5 × 10-2 μg/mL with a correlation coefficient (r) greater than 0.999. The detection (LOD) and quantification (LOQ) limits found are 1.97 × 10-3 μg/mL and 5.48 × 10-3 μg/mL respectively. Recovery is achieved with 99.9% and 100.3% trueness, intra-day precision with a coefficient of variation of repeatability (CVr) of 0.99% and inter-day precision with a coefficient of variation of precision (CVR) of 1.7%. The method has been successfully applied in the analysis of 10 batches of nevirapine tablets and suspensions.

A new production component method for natural gas development planning

Based on an analysis of the limitations of conventional production component methods for natural gas development planning,this study proposes a new one that uses life cycle models for the trend fitting and prediction of production.In this new method,the annual production of old and new wells is predicted by year first and then is summed up to yield the production for the planning period.It shows that the changes in the production of old wells in old blocks can be fitted and predicted using the vapor pressure model(VPM),with precision of 80%e95%,which is 6.6%e13.2%higher than that of other life cycle models.Furthermore,a new production prediction process and method for new wells have been established based on this life cycle model to predict the production of medium-to-shallow gas reservoirs in western Sichuan Basin,with predication error of production rate in 2021 and 2022 being 6%and 3%respectively.The new method can be used to guide the medium-and long-term planning or annual scheme preparation for gas development.It is also applicable to planning for large single gas blocks that require continuous infill drilling and adjustment to improve gas recovery.

Agile Development Methods in Software Engineering and Their Efficiency Analysis

This paper delves into Agile Development Methods in Software Engineering,contrasting them with the traditional Waterfall model and analyzing their efficiency.Agile methods,known for their adaptability and customer-centric approach,have gained prominence in the fast-paced software development industry.These methods,including Scrum,Kanban,and Extreme Programming(XP),are characterized by iterative cycles,collaborative efforts,and a focus on rapid delivery and quality improvement.The paper compares these agile methodologies to the sequential and rigid Waterfall model,highlighting agile’s superior flexibility,adaptability,and responsiveness to changing requirements.It emphasizes the importance of customer involvement in agile processes,which leads to higher satisfaction and better alignment with user expectations.The analysis reveals that agile methods not only enhance the speed of delivery but also improve the overall quality of the software product.The paper concludes that agile methodologies are more effective in today's dynamic software development environment,providing a robust framework for managing complex projects and ensuring the delivery of high-quality,relevant software solutions.

Construction of the Curriculum System of Software Engineering Based on the Agile Development Method

Under the background of“new engineering”construction,software engineering teaching pays more attention to cultivating students’engineering practice and innovation ability.In view of the inconsistency between development and demand design,team division of labor,difficult measurement of individual contribution,single assessment method,and other problems in traditional practice teaching,this paper proposes that under the guidance of agile development methods,software engineering courses should adopt Scrum framework to organize course project practice,use agile collaboration platform to implement individual work,follow up experiment progress,and ensure effective project advancement.The statistical data of curriculum“diversity”assessment show that there is an obvious improvement effect on students’software engineering ability and quality.

From Knowledge Transfer to Capability Development:The Future of PBL+CBL Teaching Method in Operating Room Nursing Education

Concomitant with the advancement of contemporary medical technology,the significance of perioperative nursing has been increasingly accentuated,necessitating elevated standards for the pedagogy of perioperative nursing.Presently,the PBL(problem-based learning)pedagogical approach,when integrated with CBL(case-based learning),has garnered considerable interest.An extensive literature review has been conducted to analyze the application of the PBL-CBL fusion in the education of perioperative nursing.Findings indicate that this integrative teaching methodology not only enhances students’theoretical knowledge,practical competencies,and collaborative skills but also contributes to the elevation of teaching quality.In conclusion,the PBL-CBL teaching approach holds immense potential for broader application in perioperative nursing education.Nevertheless,it is imperative to continually refine this combined pedagogical strategy to further enhance the caliber of perioperative nursing instruction and to cultivate a greater number of exceptional nursing professionals in the operating room setting.

Validation and Evaluation of a Mechanistic Model of Phasic and Phenological Development in Wheat

Three sets of data from the field experiments with different wheat( Triticum L. ) varieties and sowing dates in China and USA were used to test the performance of the mechanistic model of wheat development. The results showed that the absolute prediction errors for most phasic and phenological stages ranged within 0 - 5 days, and the root mean square errors were generally less than 5 days. The model was of high accuracy and low error especially for emergence, tillering, stamen and pistil initiation, and heading stages, reflecting an enhanced level of mechanism and prediction.