scholarly journals Azocasein Substrate for Determination of Proteolytic Activity: Reexamining a Traditional Method Using Bromelain Samples

2016 ◽  
Vol 2016 ◽  
pp. 1-6 ◽  
Author(s):  
Diego F. Coêlho ◽  
Thais Peron Saturnino ◽  
Fernanda Freitas Fernandes ◽  
Priscila Gava Mazzola ◽  
Edgar Silveira ◽  
...  
Keyword(s):  
Quality Control ◽  
Traditional Method ◽  
Reliable Method ◽  
Limit Of Detection ◽  
Standard Protocol ◽  
Mathematical Approach ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Selection Of

Given the importance of protease’s worldwide market, the determination of optimum conditions and the development of a standard protocol are critical during selection of a reliable method to determine its bioactivity. This paper uses quality control theory to validate a modified version of a method proposed by Charney and Tomarelli in 1947. The results obtained showed that using azocasein substrate bromelain had its optimum at 45°C and pH 9 (Glycine-NaOH 100 mM). We also quantified the limit of detection (LoD) and limit of quantification (LoQ) in the above-mentioned optimum (0.072 and 0.494 mg·mL−1of azocasein, resp.) and a calibration curve that correlates optical density with the amount of substrate digested. In all analysed samples, we observed a significant decrease in response after storage (around 17%), which suggests its use must be immediately after preparation. Thus, the protocol presented in this paper offers a significant improvement, given that subjective definitions are commonly used in the literature and this simple mathematical approach makes it clear and concise.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

Reliable Method for the Determination of Food Additive by Capillary Electrophoresis Using a Microvolume of Foodstuffs

2011 ◽  
Vol 361-363 ◽  
pp. 1486-1489
Author(s):  
Qian Xiang ◽  
Ying Gao
Keyword(s):  
Capillary Electrophoresis ◽  
Reliable Method ◽  
Lower Cost ◽  
Limit Of Detection ◽  
Food Additive ◽  
Fast Method ◽  
Optimum Conditions ◽  
Applied Potential ◽  
Minimal Sample

A fast method for the separation and determination of the food additive propyl gallate has been established by using capillary electrophoresis. The effects of several factors such as the applied potential and detection running buffer were investigated in order to obtain the optimum conditions, and the assay results were satisfactory. The limit of detection for the analyte was 10-6 mol/L. This approach has remarkable advantages with respect to other methodologies involving separations and electrochemical detection including minimal sample consumption, higher analysis speed and lower cost. In order to demonstrate the capabilitiy of the method, the determination of additive in a commercial food sample is also presented.

scholarly journals Spectrophotometric Determination of Copper(II) using 2,2[O-Tolidine-4,4-bis azo]bis[4,5-diphenyl imidazole](MBBAI)

2020 ◽  
Vol 17 (1(Suppl.)) ◽  
pp. 0287
Author(s):  
Ihsan Mahdi Shaheed
Keyword(s):  
Limit Of Detection ◽  
Ph Effect ◽  
Stoichiometric Composition ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Factors Affecting ◽  
Dental Filling ◽  
Concentration Time ◽  
Determination Of Copper

            Spectrophotometric method was developed for the determination of copper(II) ion. Synthesized (2,2[O-Tolidine-4,4-bis azo]bis[4,5-diphenyl imidazole]) (MBBAI) was used as chromogenic reagent at pH=5. Various factors affecting complex formation, such as, pH effect, reagent concentration, time effect and temperature effect, have been considered and studied. Under optimum conditions concentration ranged from (5.00-80.00) µg/mL of copper(II) obeyed Beer`s Low. Maximum absorption of the complex was 409nm with molar absorpitivity 0.127x104 L mol-1 cm-1. Limit of detection(LOD) and Limit of quantification were 1.924 and 6.42 μg/mL, respectively. The stoichiometric composition of the chelate is 1:2 (Cu:MBBAI). Experimental results for studying some selected ions as interference were reported. The developed method was successfully applied to determine copper (II) ion in dental filling.  

scholarly journals Simultaneous Determination of Aspirin and Rosuvastatin Calcium in Capsules by Using RP-HPLC Coupled with Photo Diode Array Detection

2014 ◽  
Vol 33 ◽  
pp. 218-230
Author(s):  
Ankita Panchal ◽  
Gaurav Sanghvi ◽  
Ashish Vachhani ◽  
Navin Sheth ◽  
Devendra Vaishnav
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Lower Limit ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Rosuvastatin Calcium

A simple, sensitive, specific, and cost effective method for simultaneous determination of Aspirin and Rosuvastatin calcium was developed and validated in single dosage formulation. The sample solution of ASP and RSTC was prepared using methanol as a solvent. Separation of ASP and RSTC was achieved with a mobile phase consisting of 20 mM KH2PO4 : Methanol (30:70 v/v) at a flow rate of 1.0 ml/min. Separations were performed on Merck hibar 250-4.6 RP18 (5 µm) column (150 mm X 3.0 mm), using a Shimadzu Prominence HPLC system equipped with a Shimadzu SPD-20A detector, Rhenodyne 7725i injector with 20 μL loop, LC-20 AD pump, CBM-20 Alite controller and LC Solution software. Retention times of ASP and RSTC were 3.747 and 5.969 minutes respectively. Absolute recovery of ASP and RSTC was 100.3 and 100.03 % respectively. The lower limit of quantification (LLOQ) of ASP and RSTC was 0.3097 and 0.1063 ppm and lower limit of detection (LLOD) of ASP and RSTC was 0.01535 and 0.01358 ppm respectively. Linearity was established for the range of concentrations 15.00-90.0 μg/ml and 2.0-12.0 μg/ml for ASP and RSTC respectively with the coefficient of determination (R2) of 0.994 and 0.999 for both the compounds. The inter- and intra-day precision in the measurement of ASP quality control (QC) sample 75 μg/ml, were in the range 0.1-0.2 % relative standard deviation (R.S.D.) and 0.2-0.3 % R.S.D., respectively. The inter- and intra-day precision in the measurement of RST quality control (QC) sample 10 μg/ml, were in the range 0.1-0.2 % R.S.D., and 0.0-0.3 % R.S.D., respectively. The developed method would be applicable for routine quality control of ASP And RSTC in bulk as well as in pharmaceutical formulations

scholarly journals Telmisartan Quality Control by Validation of UV-Spectrophotometric Method

2016 ◽  
Vol 1 (04) ◽  
Author(s):  
Dobrina Tsvetkova ◽  
Danka Obreshkova ◽  
Stefka Ivanova ◽  
Vladimir Yankov ◽  
Peter Atanasov ◽  
...  
Keyword(s):  
Quality Control ◽  
Confidence Interval ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Accuracy And Precision ◽  
Analytical Parameter ◽  
Degree Of Recovery

The aim of current study was to validate spectrophotometric method with UV-detection for identification and determination of Telmisartan in 99.8 % ethanol in respect of analytical parameters: selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision (repeatability). For Telmisartan in 99.8 % еthanol at λ max = 298 nm for A1%1cm and ε the obtained results for А > 0.2 and А < 0.2 are: 1) А > 0.2: at 3.10–6 g/ml ÷ 1.25.10–5 g/ml; A1%1cm: 725 ÷ 823; ε: 37347 ÷ 423352) А < 0.2: at 2.5.10–7 g/ml ÷ 1.10–6 g/ml; A1%1cm: 1201 ÷ 1567; ε: 61816 ÷ 80651 Analytical parameter accuracy is represented by the degree of recovery, which in the corresponding confidence possibility suit the confidence interval: R СТ60: 100.31 % ÷ 102.05 %; R СТ80: 99.22 % ÷ 103.18 %; R СТ100 : 93.58 % ÷ 101.9 %. For precision is proved that all results for the quantities correspond to the relevant confidence interval: СТ60: 60.31 mg ÷ 60.77 mg; СТ80: 79.82 mg ÷ 82.18 mg; СТ100: 94.22 mg ÷ 101.58 mg.

scholarly journals Determination of Glibenclamide By Analytical Spectrophotometry

2021 ◽  
Vol 18 ◽  
pp. 40-48
Author(s):  
Saad Antakli ◽  
Leon Nejem ◽  
Monzer Alraii
Keyword(s):  
Quality Control ◽  
Regression Analysis ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Extraction Process ◽  
Metformin Hydrochloride ◽  
Limit Of Quantification ◽  
First Derivative

Simple and rapid spectrophotometric method was developed and applied to determine Glibenclamide (GB) by zero spectrophotometric method and first derivative spectrophotometric method for determining of (GB) in the presence of Metformin hydrochloride (MET). Zero spectrophotometric (ZS) method was applied for the determination of (GB) at λmax = 300 nm. Linearity range was (4 – 360) μg/mL. Regression analysis showed a good correlation coefficients R2 = 0.99993. The limit of detection (LOD) and limit of quantification (LOQ) were to be 0.65 μg/mL and 2.31 μg/mL, respectively.  First derivative spectrophotometric (1DS) method was applied for the determination of (GB) in the presence (MET). (GB) was determined at 317 nm (1D317). Linearity ranges were (4 – 240) μg/mL for (GB). Regression analysis showed a good correlation coefficients R2 = 0.999914. The limit of detection (LOD) and limit of quantification (LOQ) were to be 0.60 μg/mL and 1.83 μg/mL for (GB). The proposed zero spectrophotometry method was applied to analysis individual (GB), and the derivative (1D317) method was applied to analysis (GB) individually or combined with (MET) in Syrian trademark drugs. The proposed method is simple, direct, sensitive and do not require any extraction process. Thus, this method could be readily applicable for the quality control and routine analysis.

scholarly journals Simultaneous determination of chloramphenicol and hydrocortisone acetate in cream using TLC desitrometry method

2012 ◽  
Vol 2 (1) ◽  
pp. 7-10 ◽  
Author(s):  
Nia Kristiningrum ◽  
Mia Rakhmawati
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
Hydrocortisone Acetate ◽  
Limit Of Quantification ◽  
Quality Control Testing ◽  
Label Claim ◽  
Routine Quality Control

A rapid and reproducible TLC method was developed for the determination of hydrocortisone acetate and chloramphenicol in cream. The analytes were dissolved with methanol and chromatographed on silica Gel GF 254 TLC plate using chloroform:ethyl acetate in the ratio of 1:1.5 (v/v) as mobile phase. Spots at Rf 0.29 and Rf 0.59 were recognized as chloramphenicol and hydrocortisone acetate, respectively. Quantitative analysis was done through densitometric measurement at wavelength 265 nm. Method was found linear over the concentration range of 300-900 ng/spot with the correlation coefficient of 0.999 and 0.998 for hydrocortisone acetate and chloramphenicol, respectively. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 23.84 and 71.51 ng/spot for hydrocortisone acetate, 21.06 and 63.18 ng/spot for chloramphenicol. The precision of this method was less than 2.8% whereas the means of the recovery data were 100.40± 0.579% for hydrocortisone acetate and 100.24±1.20% for chloramphenicol. The proposed method has been applied to the determination of hydrocortisone acetate and chloramphenicol in commercial cream formulations and the recovery of label claim were 99.23±0.66% (chloramphenicol) and 99.25±0.41% (hydrocortisone acetate) for brand A and 100.32±0.87% (chloramphenicol) and 100.53±0.78% (hydrocortisone acetate) for brand B. The developed method was successfully used for the assay of hydrocortisone acetate and chloramphenicol. The method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v2i1.12871 International Current Pharmaceutical Journal 2012, 2(1): 7-10 

scholarly journals Determination of the limit of quantification of the calorimeter using a mixture of benzoic acid and silicon dioxide

2011 ◽  
Vol 65 (1) ◽  
pp. 93-97
Author(s):  
Vesna Krstic ◽  
Branko Blagojevic ◽  
Lidija Gomidzelovic ◽  
Emina Pozega ◽  
Jelena Petrovic ◽  
...  
Keyword(s):  
Quality Control ◽  
Benzoic Acid ◽  
Silicon Dioxide ◽  
Limit Of Detection ◽  
Certified Reference Materials ◽  
Laboratory Work ◽  
Measuring Range ◽  
Limit Of Quantification ◽  
Detection And Quantification

In recent years quality control has received a great attention in laboratory work. Implementation of the international standard ISO/IEC 17025 is necessary for any laboratory that wishes to establish quality control in its work. One of the important factors for meeting the requirements of this standard is the usage of the certified reference materials (CRM) in laboratory work. In order to determine the performance of the calorimeter, benzoic acid as CRM, from AlliedSignal Riedelda Haen, Ref.: 33045 and SiO2, Pro analyze, in various mass ratios was used. The results showed that benzoic acid can be successfully utilized for the control of the entire technical and instrumental measuring range and resolve the problem of determination of the limit of detection and quantification of the calorimeter.

scholarly journals Determination of Tetracycline in Capsule Dosage Form

2020 ◽  
Vol 10 (03) ◽  
pp. 465-467
Author(s):  
Ali N. Hussein ◽  
Ahmed M. J. Jehan Yin ◽  
Murtada M. Hasan
Keyword(s):  
Dosage Form ◽  
Reliable Method ◽  
Limit Of Detection ◽  
Standard Addition ◽  
Tetracycline Hydrochloride ◽  
Addition Method ◽  
Limit Of Quantification ◽  
Uv Visible ◽  
Day By Day

Background: Tetracycline antibiotic is widely prescribed that encourages the finding of rapid and reliable protocol for the determination of tetracycline hydrochloride in hard gelatine capsules. Recently, the standard addition method is used commonly with the aid of a UV-visible (UV-vis) spectrophotometer for such purpose. In this work, the authors aim to quantify the percent assay of Apcycline-250 capsules utilizing the standard addition protocol. Methods: Twenty filled and emptied capsules were weighed and an equivalent amount of 50 mg of tetracycline hydrochloride was diluted, filtered, and an appropriate standard was spiked and prepared for assay. Results: The λmax was found to be 348 nm and the absorbance vs. concentration standard addition curve was plotted for tetracycline hydrochloride capsules. This curve shows good linearity (R2 = 0.9994). The limit of detection (LoD) and limit of quantification (LoQ) were observed as 0.007937 and 0.02646, respectively. While the percent assay was 103.2%. Conclusion: The authors conclude that the standard addition technique is a reliable method to conduct rapid, economical, and validated day-by-day analyses work of tetracycline hydrochloride hard gelatine capsules.

scholarly journals Spectrophotometric determination of ranitidine hydrochloride (RNH) in pharmaceutical formulation using 9-fluorenylmethyl chloroformate (FMOC-Cl)

2018 ◽  
Vol 6 (6) ◽  
pp. 7-14
Author(s):  
Abdalla Ahmed Elbashir ◽  
Shahd Moutasim Merghani
Keyword(s):  
Quality Control ◽  
Absorption Maximum ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Reaction Conditions ◽  
Limit Of Quantification ◽  
Ranitidine Hydrochloride ◽  
Ich Guidelines ◽  
Sensitive Spectrophotometric Method

A new, simple and sensitive spectrophotometric method is developed for the determination of ranitidine hydrochloride (RNH). The proposed method is based upon reaction of RNH with 9-fluorenylmethyl chloroformate (FMOC-Cl) in borate buffer of pH 8.0 producing an absorption maximum at 255 nm. All parameters required for the reaction conditions are investigated. Linearity is verified with a range of 2-16 μg/mL and is described by the regression equation y = 61129 x + 0.0354 with a correlation coefficient of 0.9998 (n = 7). The limit of detection (LOD) and the limit of quantification (LOQ) were calculated as per ICH guidelines and were found to be 0.2219 and 0.6724 μg/mL, respectively. The method was successfully applied for the determination of RNH in pharmaceutical formulation. Therefore, the method can be used for routine analysis of RNH in quality control laboratories.

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