Pub Date : 2022-07-07DOI: 10.26420/austinjanalpharmchem.2022.1145
Hossain Mm, Hanna Asma, Kamal Mm, Hossain Ma, Zaman S
The study was undertaken to assess the quality of broiler meat via detection of heavy metal contents. Seven farms were selected randomly from the five divisions of Bangladesh. Broiler meat samples were collected during starting and growing phases of production stage from each of the farms by purchasing to detect the heavy metal contents i.e chromium (Cr) and cadmium (Cd) in this study. A total of 210 meat samples (105 starter and 105 grower) was collected from the selected farms and analyzed to determine the concentration of toxic metals (Cr, Cd) in meat samples. The heavy metal data (Cr, Cd) of broiler starter meat samples from laboratory analyses of five divisions of seven feed mills were unaffected (P>0.05) between treatment. The Cd contents of broiler grower meat samples of five divisions of seven farms together differed significantly (P<0.05) between treatment except for Cr. Significant variation (P<0.01) was observed in the various meat samples of broiler chicken by individual division (Dhaka, Chittagomg). It can be concluded that the quality of broiler meat of different farms appears to be good based on the chemical evaluation, even though variation was found in the toxic metal contents of meat samples. The analyzed concentration of toxic metals in meat samples were within the range or limits of the acceptable level, so no possibility of causing health hazard will create over the consumer world through after consumption of broiler meat.
{"title":"Evaluation of Broiler Meat through Detection of Poisonous Metals (Cr, Cd) Available in Bangladesh","authors":"Hossain Mm, Hanna Asma, Kamal Mm, Hossain Ma, Zaman S","doi":"10.26420/austinjanalpharmchem.2022.1145","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1145","url":null,"abstract":"The study was undertaken to assess the quality of broiler meat via detection of heavy metal contents. Seven farms were selected randomly from the five divisions of Bangladesh. Broiler meat samples were collected during starting and growing phases of production stage from each of the farms by purchasing to detect the heavy metal contents i.e chromium (Cr) and cadmium (Cd) in this study. A total of 210 meat samples (105 starter and 105 grower) was collected from the selected farms and analyzed to determine the concentration of toxic metals (Cr, Cd) in meat samples. The heavy metal data (Cr, Cd) of broiler starter meat samples from laboratory analyses of five divisions of seven feed mills were unaffected (P>0.05) between treatment. The Cd contents of broiler grower meat samples of five divisions of seven farms together differed significantly (P<0.05) between treatment except for Cr. Significant variation (P<0.01) was observed in the various meat samples of broiler chicken by individual division (Dhaka, Chittagomg). It can be concluded that the quality of broiler meat of different farms appears to be good based on the chemical evaluation, even though variation was found in the toxic metal contents of meat samples. The analyzed concentration of toxic metals in meat samples were within the range or limits of the acceptable level, so no possibility of causing health hazard will create over the consumer world through after consumption of broiler meat.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44032459","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-06-27DOI: 10.26420/austinjanalpharmchem.2022.1144
Debnath Manika, Abrham Ayele
Objective: The study presents the validation protocol for the determination of total phosphorus content at parts per million (ppm) (μg/L) levels in animal feed by a UV-Vis spectrophotometer. Methods: The measured absorbance of solutions against the blank solution was at 400 nm with the spectrophotometer. A combined ammonium heptamolybdate tetrahydrate and ammonium monovanadate blue solution was used as a coloring reagent for detection. This method was validated by evaluation of statistical parameters such as linearity, sensitivity, limits of detection (LOD) and quantification (LOQ), precision, accuracy, and measurement uncertainty using a matrix blank (MB) against the phosphorus standard. Results: The Instrumental Detection Limit was 0.066 ppm and the Instrumental Quantification Limit was 0.22 ppm, respectively, while the phosphorus recovery and repeatability percent were 101.15% and 0.11%, respectively. However, the linearity of this method was 0.1 to 30 ppm. The measurement uncertainty of this method was 2.82%, following Commission Regulation (EC). Conclusion: The estimated parameters in the validation protocol, were found to meet the imposed performance criteria, and the procedure was validated for the intended use.
{"title":"Method Validation and Uncertainty Estimation for Total Phosphorus Determination in Animal Feed Using UV-Vis Spectrophotometer","authors":"Debnath Manika, Abrham Ayele","doi":"10.26420/austinjanalpharmchem.2022.1144","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1144","url":null,"abstract":"Objective: The study presents the validation protocol for the determination of total phosphorus content at parts per million (ppm) (μg/L) levels in animal feed by a UV-Vis spectrophotometer. Methods: The measured absorbance of solutions against the blank solution was at 400 nm with the spectrophotometer. A combined ammonium heptamolybdate tetrahydrate and ammonium monovanadate blue solution was used as a coloring reagent for detection. This method was validated by evaluation of statistical parameters such as linearity, sensitivity, limits of detection (LOD) and quantification (LOQ), precision, accuracy, and measurement uncertainty using a matrix blank (MB) against the phosphorus standard. Results: The Instrumental Detection Limit was 0.066 ppm and the Instrumental Quantification Limit was 0.22 ppm, respectively, while the phosphorus recovery and repeatability percent were 101.15% and 0.11%, respectively. However, the linearity of this method was 0.1 to 30 ppm. The measurement uncertainty of this method was 2.82%, following Commission Regulation (EC). Conclusion: The estimated parameters in the validation protocol, were found to meet the imposed performance criteria, and the procedure was validated for the intended use.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-06-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46012705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-05-25DOI: 10.26420/austinjanalpharmchem.2022.1143
Hosain Mz, Islam Sms, Kamal Mm, Rahman Mm
Quantification of vitamins in complex matrices such as feed additives is a time-consuming analytical procedure. In this study, a simple and precise in-house High Performance Liquid Chromatography (HPLC) method was developed and validated for the simultaneous detection and quantification of four fat-soluble vitamins such as vitamin A, D3 , E, and K3 in feed additives. The HPLC method was developed and validated using reversed-phase column chromatography. The chromatographic separation of the vitamins was carried out at 25° C temperature on a reverse-phase C18 column using a binary gradient pump mode. Mobile phase constituents were solvent (a): deionized water and (b) methanol. Detection was performed with HPLC ultraviolet/visible detection set at 325, 265, 230, and 254 nm wavelength for vitamin A, D3 , E, and K3 respectively. The flow rate was 1.0mL/min and the total run time was 20min. The method was validated according to the guidelines of the International Conference on Harmonization (ICH) and Food and Drug Administration (FDA), USA, and acceptance criteria for system suitability, specificity, linearity, accuracy, and precision were met in all the cases. The Relative Standard Deviation (RSD) for system suitability and precision was <2% for all the studied vitamins. The linearity of the calibration curves was excellent (R2 >0.999) at concentrations of 2.5, 5.0, 7.5, 10.0, 15.0, and 20.0 µg/mL for all vitamins, and the range of linearity of this method was 0.0-50.0 μg/mL with R2 value greater than 0.999. The limits of detection values were 0.0022, 0.0012, 0.0022, and 0.0020 µg/ mL for vitamin A, D3 , E, and K3 , respectively, and the limits of quantification values were 0.0066, 0.0038, 0.0066, and 0.0061 µg/mL for vitamin- A, D3 , E, and K3 respectively. The recovery percentages ranged from 85% to 103%, and the robustness of the method is also high with excellent reproducibility. The overall parameters of the proposed method met the validation criteria and this method could be a precise and highly desirable analytical procedure for accurate quantification of four fat-soluble vitamins such as A, D3 , E, and K3 in feed additives using a single chromatographic run.
{"title":"Quantitative Analysis of Fat-Soluble Vitamins in Feed Additives Using an In-House Developed and Validated HPLC Method","authors":"Hosain Mz, Islam Sms, Kamal Mm, Rahman Mm","doi":"10.26420/austinjanalpharmchem.2022.1143","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1143","url":null,"abstract":"Quantification of vitamins in complex matrices such as feed additives is a time-consuming analytical procedure. In this study, a simple and precise in-house High Performance Liquid Chromatography (HPLC) method was developed and validated for the simultaneous detection and quantification of four fat-soluble vitamins such as vitamin A, D3 , E, and K3 in feed additives. The HPLC method was developed and validated using reversed-phase column chromatography. The chromatographic separation of the vitamins was carried out at 25° C temperature on a reverse-phase C18 column using a binary gradient pump mode. Mobile phase constituents were solvent (a): deionized water and (b) methanol. Detection was performed with HPLC ultraviolet/visible detection set at 325, 265, 230, and 254 nm wavelength for vitamin A, D3 , E, and K3 respectively. The flow rate was 1.0mL/min and the total run time was 20min. The method was validated according to the guidelines of the International Conference on Harmonization (ICH) and Food and Drug Administration (FDA), USA, and acceptance criteria for system suitability, specificity, linearity, accuracy, and precision were met in all the cases. The Relative Standard Deviation (RSD) for system suitability and precision was <2% for all the studied vitamins. The linearity of the calibration curves was excellent (R2 >0.999) at concentrations of 2.5, 5.0, 7.5, 10.0, 15.0, and 20.0 µg/mL for all vitamins, and the range of linearity of this method was 0.0-50.0 μg/mL with R2 value greater than 0.999. The limits of detection values were 0.0022, 0.0012, 0.0022, and 0.0020 µg/ mL for vitamin A, D3 , E, and K3 , respectively, and the limits of quantification values were 0.0066, 0.0038, 0.0066, and 0.0061 µg/mL for vitamin- A, D3 , E, and K3 respectively. The recovery percentages ranged from 85% to 103%, and the robustness of the method is also high with excellent reproducibility. The overall parameters of the proposed method met the validation criteria and this method could be a precise and highly desirable analytical procedure for accurate quantification of four fat-soluble vitamins such as A, D3 , E, and K3 in feed additives using a single chromatographic run.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45480337","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-05-25DOI: 10.26420/austinjanalpharmchem.2022.1142
Hossain Mm, Hanna Asma, Kamal Mm, Hossain Ma, Zaman S
Milk is considered as an ideal food item, and it can be contaminated with the toxic metal (Pb) by various ways. The metal lead (Pb) exposes toxicity greatly when it accumulates gradually inside the body cavity of human or animal. The study is aimed at the detection of poisonous mineral lead in cow’s milk sample by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS) method.Besides, public health concern or issues in the food chain of the consumer world is also taken into consideration in this study. Though the method is a bit troublesome, but an attempt was made herein this study to make it easy access for the determination and method validation for the analysis of mineral content in milk sample by complying with the Council Directive 333/2007/E. For the ratification of this method, a pretty good number of criteria including linear range, limits of detection and quantifications, accuracy (%), measuring uncertainty, repeatability and reproducibility or precision checks etc., were assessed for the affirmation of the method. GF-AAS (Model: AA-7000 Shimadzu, Japan) technique was used for the analysis of poisonous element lead in dairy cow milk samples. Lastly, detection of Pb in milk samples was done with ultraviolet/visible detection set at 283.0 nm wave length. The method was confirmed complying with the international guidelines and acceptance values for system suitability, precision, linearity, uncertainty and accuracy or recovery % were met in all aspects. The Relative Standard Deviation (RSD) or Coefficient of Variation (CV%) for system suitability and precision was <10% for the metal (Pb) measured in the milk sample. The linearity of the calibration curves was excellent (r2>0.999) at various concentrations for the lead. The instrumental Limits of Detection (LoD) value in milk were 0.397 and the limits of quantification (LoQ) value in milk samples was 1.32μg//L, respectively, for Pb, And the method of LoD and LoQ for Pb being 0.993 and 3.30 μg/Kg, respectively. The overall recovery (%) found 98.98 for the metal (Pb). The overall RSD or CV% of reproducibility and repeatability percentages being 6.85 and 7.65%, respectively. The value for measurement uncertainty (%) was 7.0 for Pb. The developed validated parameters denote that it is an easy and economical method that can be applied greatly for the regular laboratory analysis of trace mineral element in cow milk samples. After all, the potential health of the consumer health or public health concern should not be ignored at all for the continual ingestion of toxic element contained in the milk, even though the toxic mineral content found in the supplied milk samples were within the acceptable range.
{"title":"Development and Ratification of a Precise Method (GF-AAS) Used for the Determination of Poisonous Metal Lead (Pb) in Dairy Cow Milk Sample Commonly Available in the Market of Bangladesh","authors":"Hossain Mm, Hanna Asma, Kamal Mm, Hossain Ma, Zaman S","doi":"10.26420/austinjanalpharmchem.2022.1142","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1142","url":null,"abstract":"Milk is considered as an ideal food item, and it can be contaminated with the toxic metal (Pb) by various ways. The metal lead (Pb) exposes toxicity greatly when it accumulates gradually inside the body cavity of human or animal. The study is aimed at the detection of poisonous mineral lead in cow’s milk sample by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS) method.Besides, public health concern or issues in the food chain of the consumer world is also taken into consideration in this study. Though the method is a bit troublesome, but an attempt was made herein this study to make it easy access for the determination and method validation for the analysis of mineral content in milk sample by complying with the Council Directive 333/2007/E. For the ratification of this method, a pretty good number of criteria including linear range, limits of detection and quantifications, accuracy (%), measuring uncertainty, repeatability and reproducibility or precision checks etc., were assessed for the affirmation of the method. GF-AAS (Model: AA-7000 Shimadzu, Japan) technique was used for the analysis of poisonous element lead in dairy cow milk samples. Lastly, detection of Pb in milk samples was done with ultraviolet/visible detection set at 283.0 nm wave length. The method was confirmed complying with the international guidelines and acceptance values for system suitability, precision, linearity, uncertainty and accuracy or recovery % were met in all aspects. The Relative Standard Deviation (RSD) or Coefficient of Variation (CV%) for system suitability and precision was <10% for the metal (Pb) measured in the milk sample. The linearity of the calibration curves was excellent (r2>0.999) at various concentrations for the lead. The instrumental Limits of Detection (LoD) value in milk were 0.397 and the limits of quantification (LoQ) value in milk samples was 1.32μg//L, respectively, for Pb, And the method of LoD and LoQ for Pb being 0.993 and 3.30 μg/Kg, respectively. The overall recovery (%) found 98.98 for the metal (Pb). The overall RSD or CV% of reproducibility and repeatability percentages being 6.85 and 7.65%, respectively. The value for measurement uncertainty (%) was 7.0 for Pb. The developed validated parameters denote that it is an easy and economical method that can be applied greatly for the regular laboratory analysis of trace mineral element in cow milk samples. After all, the potential health of the consumer health or public health concern should not be ignored at all for the continual ingestion of toxic element contained in the milk, even though the toxic mineral content found in the supplied milk samples were within the acceptable range.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43299044","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-03-24DOI: 10.26420/austinjanalpharmchem.2022.1141
Salem M, Ayyad R, S. H, Gaafer A
In this work we synthesized new derivatives from Phenyl Hydrazine and series of different Aldehydes (derivatives of benzylidenes). The synthesized compounds contain different aromatic Aldehydes which attached by Benzene ring via Hydrazine moiety. These derivatives were characterized by TLC, melting points, Infrared Red, Proton Nuclear Magnetic Resonance, Carbon Thirteen Nuclear Magnetic Resonance and Mass Spectroscopy. Finally, these synthesized derivatives were tested for antiproliferative activity against multiple normal and cancerous cell lines, HepG2 (Liver Cancer) and MCF-7 (Breast Cancer) cell lines were used for cytotoxic assay.
{"title":"Design and Synthesis of New Compounds Derived from Phenyl Hydrazine and Different Aldehydes as Anticancer Agents","authors":"Salem M, Ayyad R, S. H, Gaafer A","doi":"10.26420/austinjanalpharmchem.2022.1141","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1141","url":null,"abstract":"In this work we synthesized new derivatives from Phenyl Hydrazine and series of different Aldehydes (derivatives of benzylidenes). The synthesized compounds contain different aromatic Aldehydes which attached by Benzene ring via Hydrazine moiety. These derivatives were characterized by TLC, melting points, Infrared Red, Proton Nuclear Magnetic Resonance, Carbon Thirteen Nuclear Magnetic Resonance and Mass Spectroscopy. Finally, these synthesized derivatives were tested for antiproliferative activity against multiple normal and cancerous cell lines, HepG2 (Liver Cancer) and MCF-7 (Breast Cancer) cell lines were used for cytotoxic assay.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48090569","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-02-28DOI: 10.26420/austinjanalpharmchem.2022.1140
P. S, B. R, K. B.
Lifitegrast is an LFA-1 antagonist, tetrahydroisoquinoline derivative, formulated as sterile eyedrops. Lifitegrast ophthalmic solution 5.0% was the first medication approved by the US FDA for treatment of the signs and symptoms of DED. We developed and validated two novel, economic, specific, and sensitive UV spectrophotometric and RP-HPLC methods for estimation of lifitegrast in bulk and dosage form. The linearity was found in the concentration range of 05-30 μg/mL in UV method (R²=0.9995) and 2-12 μg/mL in HPLC method (R²=0.999) with good correlation coefficient. The LOD and LOQ were found to be 0.77 μg/mL and 2.33 μg/mL, respectively by UV method. RP-HPLC method was developed at SunFire C 18 column (250 × 4.6 mm i.d., 5μm) using methanol, acetonitrile, and water as a mobile phase in the ratio of 20:60:20 (v/v) (pH = 2.27 adjusted with orthophosphoric acid). The LOD and LOQ were found to be 0.50 μg/mL and 1.52 μg/mL respectively by HPLC method. These developed methods were validated according to ICH (Q2 (R1)) guidelines with the following validation parameters i.e., specificity, linearity, accuracy, precision, LOD, LOQ, robustness, and ruggedness. The results of the study proved the applicability of the method in routine analysis of lifitegrast.
{"title":"A Validated Method Developed for Estimation of Lifitegrast in Bulk and Pharmaceutical Dosage Form by UV-Spectrophotometer and RP-HPLC","authors":"P. S, B. R, K. B.","doi":"10.26420/austinjanalpharmchem.2022.1140","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1140","url":null,"abstract":"Lifitegrast is an LFA-1 antagonist, tetrahydroisoquinoline derivative, formulated as sterile eyedrops. Lifitegrast ophthalmic solution 5.0% was the first medication approved by the US FDA for treatment of the signs and symptoms of DED. We developed and validated two novel, economic, specific, and sensitive UV spectrophotometric and RP-HPLC methods for estimation of lifitegrast in bulk and dosage form. The linearity was found in the concentration range of 05-30 μg/mL in UV method (R²=0.9995) and 2-12 μg/mL in HPLC method (R²=0.999) with good correlation coefficient. The LOD and LOQ were found to be 0.77 μg/mL and 2.33 μg/mL, respectively by UV method. RP-HPLC method was developed at SunFire C 18 column (250 × 4.6 mm i.d., 5μm) using methanol, acetonitrile, and water as a mobile phase in the ratio of 20:60:20 (v/v) (pH = 2.27 adjusted with orthophosphoric acid). The LOD and LOQ were found to be 0.50 μg/mL and 1.52 μg/mL respectively by HPLC method. These developed methods were validated according to ICH (Q2 (R1)) guidelines with the following validation parameters i.e., specificity, linearity, accuracy, precision, LOD, LOQ, robustness, and ruggedness. The results of the study proved the applicability of the method in routine analysis of lifitegrast.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48427047","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-25DOI: 10.26420/austinjanalpharmchem.2022.1138
A. S., Baig Ja, Afrid Hi, Waris M, A. W, Naeem A, Sidhu Ar
The goal of this research is to verify the proposed nano-silver amalgam paste electrode (Ag-nano-SPE) method to compare with a spectrophotometric technique based on derivatization with potassium periodate (KIO4 ), 2,4-dinitrophenyl hydrazine (DNP) and sodium hydroxide (NaOH) for the estimation of cefadroxil (CFDL) by square wave adsorptive stripping voltammetry (SWAV). The different parameters of both methods were optimized in detail separately and then compared their efficiency, selectivity, sensitivity and applications. The SWAV produced a reduction peak with a precise definition at -0.160 V while measuring CFDL in 0.04 molL-1 Britton–Robinson buffer at pH 4, accumulation potential (0.5 V), accumulation time (10 sec), and with stirring rate of 200 rpm. Whereas, the CFDL was measured at 515 nm (λmax) by UVVisible spectrophotometer after the derivatization by using 1.5 mL of 0.5 mM DNP, 1.5 mL of 6.52 mM KIO4 and 0.5 mL of 10 M NaOH solution at room temperature. The linear response for CFDL was found using the SWAV and spectrophotometric techniques along a linear dynamic range from 0.033 - 0.304 and 0.051 - 1.376 µM, respectively. However, the precision, detection limit and quantification limit of SWAV for CFDL in the samples and standards significantly lower (p <0.01) as compared to spectrophotometric method. This indicates that the SWAV is more sensitive and selective than the spectrophotometric technique for regular CFDL analysis.
本研究的目的是验证所提出的纳米银汞齐膏电极(Ag-nano-SPE)方法，并与基于高碘酸钾(KIO4)、2,4-二硝基苯肼(DNP)和氢氧化钠(NaOH)衍生化的分光光度法(方波吸附溶出伏安法(SWAV)测定头孢地螺醇(CFDL)的方法进行比较。分别对两种方法的不同参数进行了详细的优化，并对其效率、选择性、灵敏度和应用进行了比较。在pH为4、积累电位(0.5 V)、积累时间(10秒)、搅拌速度为200 rpm的0.04 mol -1 briton - robinson缓冲液中测量CFDL时，SWAV在-0.160 V下产生了一个精确定义的还原峰。在室温下，用1.5 mL 0.5 mM DNP、1.5 mL 6.52 mM KIO4和0.5 mL 10 M NaOH溶液衍生化后，用紫外可见分光光度计在515 nm (λmax)处测量CFDL。在0.033 ~ 0.304µM和0.051 ~ 1.376µM的线性动态范围内，采用SWAV和分光光度法测定CFDL的线性响应。然而，与分光光度法相比，swv法在样品和标准品中检测CFDL的精密度、检出限和定量限均显著降低(p <0.01)。这表明SWAV比分光光度法在常规CFDL分析中具有更高的灵敏度和选择性。
{"title":"Analytical Comparison of Cefadroxil Determination by Square Wave Adsorptive Stripping Voltammetric and Spectrophotometric Methods","authors":"A. S., Baig Ja, Afrid Hi, Waris M, A. W, Naeem A, Sidhu Ar","doi":"10.26420/austinjanalpharmchem.2022.1138","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2022.1138","url":null,"abstract":"The goal of this research is to verify the proposed nano-silver amalgam paste electrode (Ag-nano-SPE) method to compare with a spectrophotometric technique based on derivatization with potassium periodate (KIO4 ), 2,4-dinitrophenyl hydrazine (DNP) and sodium hydroxide (NaOH) for the estimation of cefadroxil (CFDL) by square wave adsorptive stripping voltammetry (SWAV). The different parameters of both methods were optimized in detail separately and then compared their efficiency, selectivity, sensitivity and applications. The SWAV produced a reduction peak with a precise definition at -0.160 V while measuring CFDL in 0.04 molL-1 Britton–Robinson buffer at pH 4, accumulation potential (0.5 V), accumulation time (10 sec), and with stirring rate of 200 rpm. Whereas, the CFDL was measured at 515 nm (λmax) by UVVisible spectrophotometer after the derivatization by using 1.5 mL of 0.5 mM DNP, 1.5 mL of 6.52 mM KIO4 and 0.5 mL of 10 M NaOH solution at room temperature. The linear response for CFDL was found using the SWAV and spectrophotometric techniques along a linear dynamic range from 0.033 - 0.304 and 0.051 - 1.376 µM, respectively. However, the precision, detection limit and quantification limit of SWAV for CFDL in the samples and standards significantly lower (p <0.01) as compared to spectrophotometric method. This indicates that the SWAV is more sensitive and selective than the spectrophotometric technique for regular CFDL analysis.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43095193","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2021-12-14DOI: 10.26420/austinjanalpharmchem.2021.1137
Makhdoom Hs, Saeed A, Saleem F, S. K., M. M
A reversed-phase liquid chromatographic method for ivabradine hydrochloride using Diode Array Detector (DAD) and internal standard technique was developed and validated according to ICH and SWGTOX guidelines. The prime objective of this study was to develop a precise and accurate method that can be equally applicable to biological (plasma) as well as non-biological (active pharmaceutical ingredient and pharmaceutical tablets) matrices. Losartan potassium was used as an internal standard due to its easy availability. After liquid-liquid extraction using acetonitrile, the ivabradine hydrochloride and internal standard were chromatographed on Agilent 1200 series HPLC system equipped with DAD detector, auto-sampler and chemstation software. Analytical separation was achieved on Agilent C-18 (5µm, 25cm x 4.6mm) reversed-phase column at 30°C column oven temperature, 10μL injection volume and 286nm wavelength. Isocratic mobile phase system comprised of 60:40 v/v ratio of HPLC grade methanol and water adjusted to pH 6.8 using orthophosphoric acid was employed with 1mL/min flow rate. The method linear range was 0.025-3µg/mL (25-3000ng/mL) for pharmaceutical tablets and plasma with the coefficient of linearity ranged 0.997-0.999. Results for precision, accuracy, recovery, stability and matrix effect studies were within acceptable limits for both plasma and tablets. Method was successfully applied to the commercial tablet products and patient plasma samples to estimate the amount of ivabradine hydrochloride.
根据ICH和SWGTOX指南，采用二极管阵列检测器（DAD）和内标技术开发并验证了盐酸伊伐布雷定的反相液相色谱法。本研究的主要目的是开发一种精确准确的方法，该方法同样适用于生物（血浆）和非生物（活性药物成分和片剂）基质。氯沙坦钾因其易得性而被用作内标。用乙腈液-液萃取后，在配备DAD检测器、自动采样器和chemstation软件的安捷伦1200系列高效液相色谱系统上对盐酸伊伐布雷定和内标物进行色谱分析。在Agilent C-18（5µm，25cm x 4.6mm）反相柱上，在30°C柱烘箱温度、10μL进样体积和286nm波长下实现分析分离。采用由60:40v/v比例的HPLC级甲醇和水组成的等色谱流动相系统，用正磷酸将pH调节至6.8，流速为1mL/min。片剂和血浆的方法线性范围为0.025-3µg/mL（25-3000ng/mL），线性系数为0.997-0.999。血浆和片剂的精密度、准确度、回收率、稳定性和基质效应研究结果均在可接受的限度内。方法成功地应用于商业片剂产品和患者血浆样品中盐酸伊伐布雷定的含量估算。
{"title":"Reversed-Phase Liquid Chromatographic Internal Standard Method Using Losartan Potassium for Quantitative Estimation of Ivabradine Hydrochloride in Pharmaceutical Tablet Dosage Form and Plasma","authors":"Makhdoom Hs, Saeed A, Saleem F, S. K., M. M","doi":"10.26420/austinjanalpharmchem.2021.1137","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2021.1137","url":null,"abstract":"A reversed-phase liquid chromatographic method for ivabradine hydrochloride using Diode Array Detector (DAD) and internal standard technique was developed and validated according to ICH and SWGTOX guidelines. The prime objective of this study was to develop a precise and accurate method that can be equally applicable to biological (plasma) as well as non-biological (active pharmaceutical ingredient and pharmaceutical tablets) matrices. Losartan potassium was used as an internal standard due to its easy availability. After liquid-liquid extraction using acetonitrile, the ivabradine hydrochloride and internal standard were chromatographed on Agilent 1200 series HPLC system equipped with DAD detector, auto-sampler and chemstation software. Analytical separation was achieved on Agilent C-18 (5µm, 25cm x 4.6mm) reversed-phase column at 30°C column oven temperature, 10μL injection volume and 286nm wavelength. Isocratic mobile phase system comprised of 60:40 v/v ratio of HPLC grade methanol and water adjusted to pH 6.8 using orthophosphoric acid was employed with 1mL/min flow rate. The method linear range was 0.025-3µg/mL (25-3000ng/mL) for pharmaceutical tablets and plasma with the coefficient of linearity ranged 0.997-0.999. Results for precision, accuracy, recovery, stability and matrix effect studies were within acceptable limits for both plasma and tablets. Method was successfully applied to the commercial tablet products and patient plasma samples to estimate the amount of ivabradine hydrochloride.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42090226","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2021-12-03DOI: 10.26420/austinjanalpharmchem.2021.1136
Hussein Ag, Sakr Hm, M. Am, Ayyad Rr
In this work, we carry out the testing of some Benzimidazole derivatives as anti-inflammatory using Indomethacin 10mg/Kg, diclofenac sodium 7mg/ Kg, celecoxib 100mg/Kg and tested compounds of 200mg/Kg. The tested compounds showed anti-inflammatory activity in comparison with the standard reference drugs. In additionally, carrying out the testing of ulcer index for some testing compounds 600mg/Kg comparing with indomethacin 100mg/Kg, the testing revealed indomethacin causes ulcer in stomach of the testing animals, while the testing compounds no ulcerated the stomach of the testing animal.
{"title":"Ulcer Index and Anti-Inflammatory Testing of Some Benzimidazole Derivatives","authors":"Hussein Ag, Sakr Hm, M. Am, Ayyad Rr","doi":"10.26420/austinjanalpharmchem.2021.1136","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2021.1136","url":null,"abstract":"In this work, we carry out the testing of some Benzimidazole derivatives as anti-inflammatory using Indomethacin 10mg/Kg, diclofenac sodium 7mg/ Kg, celecoxib 100mg/Kg and tested compounds of 200mg/Kg. The tested compounds showed anti-inflammatory activity in comparison with the standard reference drugs. In additionally, carrying out the testing of ulcer index for some testing compounds 600mg/Kg comparing with indomethacin 100mg/Kg, the testing revealed indomethacin causes ulcer in stomach of the testing animals, while the testing compounds no ulcerated the stomach of the testing animal.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-12-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45910210","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2021-10-29DOI: 10.26420/austinjanalpharmchem.2021.1135
Madkour Lh
Up regulation of cell cycle-regulating and DNA repair genes appears to have a negative impact on recurrence-free survival in patients with papillary thyroid cancer. Furthermore, recurrence is associated with thyroid dedifferentiation. Most cases address local applications or diseases in the filtering organs, reflecting remaining challenges in systemic delivery of siRNA. Small Interfering RNA (siRNA) is a promising drug candidate, expected to have broad therapeutic potentials toward various diseases including viral infections and cancer. With recent advances in bio conjugate chemistry and carrier technology, several siRNA-based drugs have advanced to clinical trials. The difficulty in siRNA delivery is in large part due to poor circulation stability and unfavorable pharmacokinetics and bio distribution profiles of siRNA. In this research we describe the pharmacokinetics and bio distribution of siRNA Nano medicines, focusing on those reported in the past 5 years, and their pharmacological effects in selected disease models such as hepatocellular carcinoma, liver infections, and respiratory diseases. The examples discussed here will provide an insight into the current status of the art and unmet needs in siRNA delivery.
{"title":"Pharmacokinetics, Bio Distribution and Therapeutic Applications of Recently-Developed siRNA and DNA Repair Genes Recurrence","authors":"Madkour Lh","doi":"10.26420/austinjanalpharmchem.2021.1135","DOIUrl":"https://doi.org/10.26420/austinjanalpharmchem.2021.1135","url":null,"abstract":"Up regulation of cell cycle-regulating and DNA repair genes appears to have a negative impact on recurrence-free survival in patients with papillary thyroid cancer. Furthermore, recurrence is associated with thyroid dedifferentiation. Most cases address local applications or diseases in the filtering organs, reflecting remaining challenges in systemic delivery of siRNA. Small Interfering RNA (siRNA) is a promising drug candidate, expected to have broad therapeutic potentials toward various diseases including viral infections and cancer. With recent advances in bio conjugate chemistry and carrier technology, several siRNA-based drugs have advanced to clinical trials. The difficulty in siRNA delivery is in large part due to poor circulation stability and unfavorable pharmacokinetics and bio distribution profiles of siRNA. In this research we describe the pharmacokinetics and bio distribution of siRNA Nano medicines, focusing on those reported in the past 5 years, and their pharmacological effects in selected disease models such as hepatocellular carcinoma, liver infections, and respiratory diseases. The examples discussed here will provide an insight into the current status of the art and unmet needs in siRNA delivery.","PeriodicalId":91055,"journal":{"name":"Austin journal of analytical and pharmaceutical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-10-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43223948","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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