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 ...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%.展开更多
Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulat...Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulation. The drug separation was performed on Hibar-240, Li-chrosphere-100 C18 ODS (250 × 4.6 mm, 5 μm) column, at a flow rate of 1 mL/min. The mobile phase used was a mixture of methanol: potassium di-hydrogen phosphate buffer at a ratio of 70:30 v/v. The detection was carried out at a wavelength of 266 nm. The retention times of sitagliptin phosphate and metformin hydrochloride were found as 6.1 and 4.9 min respectively. Linear calibration curves with good correlation coefficients were obtained over the concentration ranges of 10 - 50 μg/mL for sitagliptin and 20 - 100 μg/mL for metformin. The limit of detection was 0.016 and 0.14 μg/mL and the limit of quantification was 0.048 and 0.42 μg/mL for sitagliptin phosphate and metformin hydrochloride respectively. Validation of the method demonstrated system selectivity, specificity, linearity, accuracy and precision. The developed method was found useful in the simultaneous analysis of sitagliptin phosphate and metformin hydrochloride in formulation.展开更多
A sensitive, precise, accurate and simple in house validated Liquid Chromatography and Tandem mass spectrometric (LC-MS/MS) analytical method was developed for the quantification of acrylamide in potato chips, a proba...A sensitive, precise, accurate and simple in house validated Liquid Chromatography and Tandem mass spectrometric (LC-MS/MS) analytical method was developed for the quantification of acrylamide in potato chips, a probable carcinogenic and neurotoxic compound in fried food items. Acrylamide was extracted and cleaned up by QuEChERS method, then analyzed by triple quadrupole mass spectrophotometer using positive electrospray-ionization mode and d3-Acrylamide internal standard. The analyte and internal standard were separated on a reversed-phase C18 column (100 × 2.0 mm, 2.5 μm) by gradient elution with water and methanol containing 0.1% formic acid as mobile phase. The analytical method was fully validated by assessment of linearity, specificity, precision, accuracy, selectivity and robustness with relative standard deviation of less than 4%. The calibration curves were found linear with correlation coefficient (r2) of 0.9997 over the concentration range 5 - 500 μg/L. The recoveries of Acrylamide in the concentration of 250, 400, and 500 μg/L were 97% to 104%. Based on the signal to noise ratio, the lower limit of detection (LOD) and lower limit of quantification (LOQ) were achieved 2.0 μg/L and 4.0 μg/L respectively. The proposed method was also applied to other available most popular 24 types of food (265 number of sample) first time in Bangladesh. The highest level of acrylamide has been found in fried products with the range of 197.04 μg/L to 114.63 μg/L, protein-rich food lies between 79.76 to 89.14 μg/L whereas baked food products exhibited less content in the range of 35.23 to 51.17 μg/L.展开更多
A rapid, sensitive, robust, rugged and linear HPLC method is developed using QbD approach and validated as per ICH for the estimation of amlodipine impurities in tablet dosage form. Phosphate buffer with triethyl amin...A rapid, sensitive, robust, rugged and linear HPLC method is developed using QbD approach and validated as per ICH for the estimation of amlodipine impurities in tablet dosage form. Phosphate buffer with triethyl amine adjusted to pH to 2.8 is used as the mobile phase and 3μ particle size C18 column of 150 mm length and 4.6 mm internal diameter is used. Using photo diode array (PDA) detector, the compounds are monitored at 340 nm. All impurities are well separated and flow Gradient has been optimized to obtain the acceptable resolution between impurities and amlodipine. Diluent was chosen, based on the impurity peak shapes and recoveries. Test concentration and injection volume have been optimized to obtain limit of quantification (LOQ) values below the reporting threshold.展开更多
The thorough investigation of nanoplastics(NPs)in aqueous environments requires efficient and expeditious quantitative analytical methods that are sensitive to environmentally relevant NP concentrations and convenient...The thorough investigation of nanoplastics(NPs)in aqueous environments requires efficient and expeditious quantitative analytical methods that are sensitive to environmentally relevant NP concentrations and convenient to employ.Optical analysis-based quantitative methods have been acknowledged as effective and rapid approaches for quantifying NP concentrations in laboratory-scale studies.Herein,we compared three commonly used optical response indicators,namely fluorescence intensity(FI),ultraviolet absorbance,and turbidity,to assess their performance in quantifying NPs.Furthermore,orthogonal experiments were conducted to evaluate the influence of various water quality parameters on the preferred indicator-based quantification method.The results revealed that FI exhibits the highest correlation coefficient(>0.99)with NP concentration.Notably,the limit of quantification(LOQ)for various types of NPs is exceptionally low,ranging from 0.0089 to 0.0584 mg/L in ultrapure water,well below environmentally relevant concentrations.Despite variations in water quality parameters such as pH,salinity,suspended solids(SS),and humic acid,a robust relationship between detectable FI and NP concentration was identified.However,an increased matrix,especially SS in water samples,results in an enhanced LOQ for NPs.Nevertheless,the quantitative method remains applicable in real water bodies,especially in drinking water,with NP LOQ as low as 0.0157–0.0711 mg/L.This exceeds the previously reported detectable concentration for 100 nm NPs at 40µg/mL using surface-enhanced Raman spectroscopy.This study confirms the potential of FI as a reliable indicator for the rapid quantification of NPs in aqueous environments,offering substantial advantages in terms of both convenience and cost-effectiveness.展开更多
文摘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%.
文摘Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulation. The drug separation was performed on Hibar-240, Li-chrosphere-100 C18 ODS (250 × 4.6 mm, 5 μm) column, at a flow rate of 1 mL/min. The mobile phase used was a mixture of methanol: potassium di-hydrogen phosphate buffer at a ratio of 70:30 v/v. The detection was carried out at a wavelength of 266 nm. The retention times of sitagliptin phosphate and metformin hydrochloride were found as 6.1 and 4.9 min respectively. Linear calibration curves with good correlation coefficients were obtained over the concentration ranges of 10 - 50 μg/mL for sitagliptin and 20 - 100 μg/mL for metformin. The limit of detection was 0.016 and 0.14 μg/mL and the limit of quantification was 0.048 and 0.42 μg/mL for sitagliptin phosphate and metformin hydrochloride respectively. Validation of the method demonstrated system selectivity, specificity, linearity, accuracy and precision. The developed method was found useful in the simultaneous analysis of sitagliptin phosphate and metformin hydrochloride in formulation.
文摘A sensitive, precise, accurate and simple in house validated Liquid Chromatography and Tandem mass spectrometric (LC-MS/MS) analytical method was developed for the quantification of acrylamide in potato chips, a probable carcinogenic and neurotoxic compound in fried food items. Acrylamide was extracted and cleaned up by QuEChERS method, then analyzed by triple quadrupole mass spectrophotometer using positive electrospray-ionization mode and d3-Acrylamide internal standard. The analyte and internal standard were separated on a reversed-phase C18 column (100 × 2.0 mm, 2.5 μm) by gradient elution with water and methanol containing 0.1% formic acid as mobile phase. The analytical method was fully validated by assessment of linearity, specificity, precision, accuracy, selectivity and robustness with relative standard deviation of less than 4%. The calibration curves were found linear with correlation coefficient (r2) of 0.9997 over the concentration range 5 - 500 μg/L. The recoveries of Acrylamide in the concentration of 250, 400, and 500 μg/L were 97% to 104%. Based on the signal to noise ratio, the lower limit of detection (LOD) and lower limit of quantification (LOQ) were achieved 2.0 μg/L and 4.0 μg/L respectively. The proposed method was also applied to other available most popular 24 types of food (265 number of sample) first time in Bangladesh. The highest level of acrylamide has been found in fried products with the range of 197.04 μg/L to 114.63 μg/L, protein-rich food lies between 79.76 to 89.14 μg/L whereas baked food products exhibited less content in the range of 35.23 to 51.17 μg/L.
文摘A rapid, sensitive, robust, rugged and linear HPLC method is developed using QbD approach and validated as per ICH for the estimation of amlodipine impurities in tablet dosage form. Phosphate buffer with triethyl amine adjusted to pH to 2.8 is used as the mobile phase and 3μ particle size C18 column of 150 mm length and 4.6 mm internal diameter is used. Using photo diode array (PDA) detector, the compounds are monitored at 340 nm. All impurities are well separated and flow Gradient has been optimized to obtain the acceptable resolution between impurities and amlodipine. Diluent was chosen, based on the impurity peak shapes and recoveries. Test concentration and injection volume have been optimized to obtain limit of quantification (LOQ) values below the reporting threshold.
基金partly supported by the National Natural Science Foundation of China(Nos.22376066 and 22076045)the Science and Technology Commission of Shanghai Municipality’s zhongYangfan Special Project(China)(No.23YF1408400)+1 种基金the Postdoctoral Innovation Talents Support Program(China)(No.BX20230123)the Fundamental Research Funds for the Central Universities(China).
文摘The thorough investigation of nanoplastics(NPs)in aqueous environments requires efficient and expeditious quantitative analytical methods that are sensitive to environmentally relevant NP concentrations and convenient to employ.Optical analysis-based quantitative methods have been acknowledged as effective and rapid approaches for quantifying NP concentrations in laboratory-scale studies.Herein,we compared three commonly used optical response indicators,namely fluorescence intensity(FI),ultraviolet absorbance,and turbidity,to assess their performance in quantifying NPs.Furthermore,orthogonal experiments were conducted to evaluate the influence of various water quality parameters on the preferred indicator-based quantification method.The results revealed that FI exhibits the highest correlation coefficient(>0.99)with NP concentration.Notably,the limit of quantification(LOQ)for various types of NPs is exceptionally low,ranging from 0.0089 to 0.0584 mg/L in ultrapure water,well below environmentally relevant concentrations.Despite variations in water quality parameters such as pH,salinity,suspended solids(SS),and humic acid,a robust relationship between detectable FI and NP concentration was identified.However,an increased matrix,especially SS in water samples,results in an enhanced LOQ for NPs.Nevertheless,the quantitative method remains applicable in real water bodies,especially in drinking water,with NP LOQ as low as 0.0157–0.0711 mg/L.This exceeds the previously reported detectable concentration for 100 nm NPs at 40µg/mL using surface-enhanced Raman spectroscopy.This study confirms the potential of FI as a reliable indicator for the rapid quantification of NPs in aqueous environments,offering substantial advantages in terms of both convenience and cost-effectiveness.
