Development of Greener and Safer Assays for Hydrochloride Drugs: Photometric Microtitration of Phenylpropanolamine Hydrochloride and Metformin Hydrochloride

2011 ◽  
Vol 361-363 ◽  
pp. 1892-1896
Author(s):  
Theerasak Rojanarata ◽  
Kwanrutai Waewsa-Nga ◽  
Parin Buacheen ◽  
Praneet Opanasopit ◽  
Tanasait Ngawhirunpat
Keyword(s):  
Silver Nitrate ◽  
Mercuric Acetate ◽  
Raw Materials ◽  
Ammonium Thiocyanate ◽  
Cost Effective ◽  
Metformin Hydrochloride ◽  
Sustainable Environment ◽  
Accuracy And Precision ◽  
Phenylpropanolamine Hydrochloride

An environmentally friendlier, safer and saver method is described for the assay of drugs as hydrochloride salts namely metformin hydrochloride and phenylpropanolamine hydrochloride via the determination of their chloride contents. In this method, an aqueous solution of drug was treated with measured excess of silver nitrate in the presence of nitric acid, followed by the determination of unreacted silver nitrate by Volhard’s method using ammonium thiocyanate titrant and iron(III) alum indicator. To minimize the reagents consumed and wastes generated, the reactions were scaled down to less than 2 mL carried out in microcentrifuge tubes and using micropipettes for the transfer of reagents. The equivalence point was determined by spectrophotometry to diminish visual errors by reading the absorbance of red iron(III) thiocyante complex at 450 nm on microplates, which quickened the measurements of multi-samples. After validation, the method showed satisfactory accuracy and precision and was successfully applied for the assay of both drugs in raw materials, giving the results comparable to the pharmacopeial methods. In addition, the proposed assay was free from the use of harsh, toxic and environmentally harmful chemicals i.e. glacial acetic acid, acetic anhydride, mercuric acetate which are employed in the USP non-aqueous titration methods. Thus, the method is considerably safer for analysts and is a cost-effective and green analytical method suitable for a sustainable environment.

scholarly journals Development, Validation and Statistical Correlation of RP–LC Methods for Determination of Atazanavir Sulfate in Capsule Dosage Form

2012 ◽  
Vol 9 (4) ◽  
pp. 1778-1787 ◽  
Author(s):  
A. Behera ◽  
D. G. Sankar ◽  
S. K. Moitra ◽  
S. C. Si
Keyword(s):  
Analytical Method ◽  
Dosage Form ◽  
Raw Materials ◽  
Cost Effective ◽  
Statistical Correlation ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Depth Study ◽  
Atazanavir Sulfate

To study the effective therapeutic bioavailability of Atazanavir Sulfate (ATV), administered singly or in combination with Ritonavir, a cost effective and rapid method is required. In order to assess an in-depth study, it is primarily thought prudent to develop an effective analytical method for estimation of ATV in marketed dosage forms. The present work is to develop a simple and precise analytical method for in depth evaluation of therapeutic efficacy of ATV. The novelty of the method shows linearity in the concentration range of 10-100 µg/mL at two wavelengths, i.e. 254 nm and 284 nm respectively. The chromatographic system consists of HiQSil C18HS column; an isocratic mobile phase consisted of methanol and tetrahydrofuran (95:5 v/v). The developed method is validated according to ICH guidelines in capsule dosage form. Validation of the developed method shows good result in range, linearity, accuracy and precision. Student’st–test was used to correlate the two methods and applied to raw materials and capsule dosage form.

scholarly journals Development and Validation of UV Spectrophotometric Method for the Determination of Cefuroxime Axetil in Bulk and Pharmaceutical Formulation

2013 ◽  
Vol 6 (1) ◽  
pp. 133-141 ◽  
Author(s):  
S. Binte Amir ◽  
M. A. Hossain ◽  
M. A. Mazid
Keyword(s):  
Spectrophotometric Method ◽  
Cost Effective ◽  
Cefuroxime Axetil ◽  
Pharmaceutical Formulation ◽  
Uv Spectrum ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Label Claim ◽  
Development And Validation

The present study was undertaken to develop and validate a simple, sensitive, accurate, precise and reproducible UV spectrophotometric method for cefuroxime axetil using methanol as solvent. In this method the simple UV spectrum of cefuroxime axetil in methanol was obtained which exhibits absorption maxima (?max) at 278 nm. The quantitative determination of the drug was carried out at 278 nm and Beer’s law was obeyed in the range of (0.80-3.60) µg/ml. The proposed method was applied to pharmaceutical formulation and percent amount of drug estimated (95.6% and 96%) was found in good agreement with the label claim. The developed method was successfully validated with respect to linearity, specificity, accuracy and precision. The method was shown linear in the mentioned concentrations having line equation y = 0.05x + 0.048 with correlation coefficient of 0.995. The recovery values for cefuroxime axetil ranged from 99.85-100.05. The relative standard deviation of six replicates of assay was less than 2%. The percent relative standard deviations of inter-day precision ranged between 1.45-1.92% and intra-day precision of cefuroxime axetil was 0.96-1.51%. Hence, proposed method was precise, accurate and cost effective.  Keywords: UV-Vis spectrophotometer; Method validation; Cefuroxime axetil; Recovery studies.  © 2013 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.   doi: http://dx.doi.org/10.3329/jsr.v6i1.14879 J. Sci. Res. 6 (1), 133-141 (2013)  

scholarly journals An Automated and High-Throughput Immunoaffinity Magnetic Bead-Based Sample Clean-Up Platform for the Determination of Aflatoxins in Grains and Oils Using UPLC-FLD

Toxins ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 583 ◽  
Author(s):  
Zhihong Xuan ◽  
Jin Ye ◽  
Bing Zhang ◽  
Li Li ◽  
Yu Wu ◽  
...  
Keyword(s):  
High Throughput ◽  
High Performance ◽  
Cost Effective ◽  
Magnetic Bead ◽  
The Novel ◽  
Analysis Method ◽  
Automated Method ◽  
Accuracy And Precision ◽  
Optimized Conditions

Sample clean-up remains the most time-consuming and error-prone step in the whole analytical procedure for aflatoxins (AFTs) analysis. Herein, an automated and high-throughput sample clean-up platform was developed with a disposable, cost-effective immunoaffinity magnetic bead-based kit. Under optimized conditions, the automated method takes less than 30 min to simultaneously purify 20 samples without requiring any centrifugation or filtering steps. When coupled to ultra-high performance liquid chromatography with fluorescence detection, this new analysis method displays excellent accuracy and precision as well as outstanding efficiency. Furthermore, an interlaboratory study was performed in six laboratories to validate the novel protocol. Mean recovery, repeatability, reproducibility, and Horwitz ratio values were within 91.9%–107.4%, 2.5%–7.4%, 2.7%–10.6%, and 0.26%–0.90, respectively. Results demonstrate that the developed sample clean-up platform is a reliable alternative to most widely adopted clean-up procedures for AFTs in cereals and oils.

scholarly journals A Versatile Liquid Chromatographic Method for the Simultaneous Determination of Metformin, Sitagliptin, Simvastatin, and Ezetimibe in Different Dosage Forms

2018 ◽  
Vol 101 (2) ◽  
pp. 401-409 ◽  
Author(s):  
Asmaa A El-Zaher ◽  
Ehab F Elkady ◽  
Hanan M Elwy ◽  
Mahmoud Abo El Makarim Saleh
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Metformin Hydrochloride ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A new LC method is introduced with the concept of its versatile application to widely used drugs from different pharmacological classes. Metformin hydrochloride (MTF), sitagliptin phosphate (SIT), simvastatin (SIM) and ezetimibe (EZB) were simultaneously determined with a simple reversed-phase LC method in which a SIT–SIM binary mixture, present in a dosage form brand, was considered central for its development. Chromatographic separation was achieved with a mobile phase of acetonitrile and 0.02 M potassium dihydrogen phosphate (pH 5.2) (77 + 23, v/v) flowing through a C18 column (BDS Hypersil, 250 × 4.6 mm, 5 µm) at 1.2 mL/min at ambient temperature. UV detection was programmed to be carried out at 210 nm for EZB, SIT, and MTF, whereas SIM was detected at 240 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory over concentration ranges 4–40 µg/mL for EZB and SIM, 0.5–50 µg/mL for SIT, and 5–500 µg/mL for MTF. Coefficients of determination were >0.99 for the four drugs. LOQs found were 0.01 µg/mL for EZB, 0.02 µg/mL for SIT, 0.2 µg/mL for MTF, and 0.02 µg/mL for SIM. The developed method is simple, rapid, accurate, precise, and suitable for the routine QC analysis of the cited drugs in pharmaceutical products by conventional HPLC systems.

scholarly journals Determination and Removal of Phosphate and Nitrate from the Ground and Surface Water at the Three Counties of Guyana

2021 ◽  
pp. 1-20
Author(s):  
Joylyn Anita Conway ◽  
Brij Bhushan Tewari
Keyword(s):  
Surface Water ◽  
Surface Waters ◽  
Natural Waters ◽  
Cost Effective ◽  
Small Scale ◽  
Transitional Metals ◽  
Sustainable Environment ◽  
Permissible Levels ◽  
The Stability

Standard analytical procedures that are based on colourimetry facilitated the determination of PO43- and NO3- in the ground and surface waters from the three (3) counties of Guyana. Phosphates and nitrates beyond their permissible levels in natural waters can pose significant threats to the aquatic environment, its inhabitants, and the health of humans and terrestrial animals. For this reason, this study aims to investigate the use of metal (nickel, cadmium, cobalt) ferrocyanides (octahedral complexes that facilitate adsorption of anions primarily on its two divalent transitional metals) as adsorbents to facilitate the removal of the aforementioned anions. Results revealed that nickel ferrocyanide is the most effective adsorbent for treating ground and surface waters that contain high levels of PO43-, while it was also the most effective adsorbent for treating surface waters that contained NO3-. Fixed volumes of water samples were treated with 50 mg, 100 mg, and 150 mg of the adsorbent. The correlation coefficient computations revealed that they were instances of both positive and negative correlations, which implied that increasing adsorbent dosage resulted in increased adsorption and other instances decreased adsorption, respectively. This occurrence went against literature, possible reasons for this are explained in detail within the discussion portion of the manuscript. Adsorption isotherms and Langmuir plots were used to facilitate adsorption studies, in various instances, the generic appearance of these isotherms was not observed, possible reasons for this occurrence are also explained in more detail within the article. Based on observations within the article, the use of cobalt ferrocyanide for treating groundwater and removing PO43- is not recommended, while cadmium ferrocyanide is not recommended to be used to facilitate the removal of NO3-, due to the possible formation of Co3(PO4)2 and Cd(NO3)2, respectively, which consequently affected the results. Technologies like those studied in this research project should be explored and studied more in-depth (particularly with regards to the stability of the adsorbents) with regards to the treating of ground and surface water supplies, to facilitate the removal of PO43- and NO3-, since the results observed, though on a small scale, can be seen to move us closer towards a green and sustainable environment, inclusive of safeguarding the health of the Worlds’ people and expanding the scope of cost-effective and simple methods that aid in the removal of anions from natural waters.

Simultaneous Determination of Metformin, Glipizide, Repaglinide, and Glimepiride or Metformin and Pioglitazone by a Validated LC Method: Application in the Presence of Metformin Impurity (1-Cyanoguanidine)

2016 ◽  
Vol 99 (4) ◽  
pp. 957-963 ◽  
Author(s):  
Asmaa A El-Zaher ◽  
Ehab F Elkady ◽  
Hanan M Elwy ◽  
Mahmoud A Saleh
Keyword(s):  
Simultaneous Determination ◽  
Potassium Dihydrogen Phosphate ◽  
Correlation Coefficients ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Products ◽  
Metformin Hydrochloride ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision

Abstract A rapid, simple, and precise RPLC method was developed for the simultaneous determination of the widely used oral antidiabetic, metformin hydrochloride (MTF), with some commonly coadministered oral antidiabetics from different pharmacological classes—glipizide (GPZ), pioglitazone hydrochloride (PGZ), glimepiride (GLM), and repaglinide (RPG)—in bulk, laboratory-prepared mixtures and pharmaceutical formulations in the presence of metformin-reported impurity [1-cyanoguanidine (CNG)]. Chromatographic separation was achieved using isocratic elution mode with a mobile phase of acetonitrile: 0.02 M potassium dihydrogen phosphate (pH 3.17; 50–50, v/v) flowing through a CN Phenomenex column (Phenosphere Next, 250 × 4.6 mm, 5 μm) at a rate of 1.5 mL/min at ambient temperature. UV detection was carried out at 220 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory for concentration ranges: 0.175–350 μg/mL for MTF, 0.0525–105 μg/mL for GPZ, 0.125–250 μg/mL for PGZ, and 0.05–100 μg/mL for GLM and RPG. Correlation coefficients were >0.99 for all analytes. LOQs were 0.009 μg/mL for MTF, 0.009 μg/mL for GPZ, 0.04 μg/mL for GLM, 0.124 μg/mL for PGZ, and 0.044 μg/mL for RPG. The developed method is specific, accurate, and suitable for the QC and routine analysis of the cited drugs in their pharmaceutical products.

scholarly journals A UV-Spectrophotmetric Chemometric Method for the Simultaneous Determination of Sulfadoxine and Pyrimethamine in Tablets

2016 ◽  
Vol 8 (3) ◽  
pp. 76
Author(s):  
Hagga M. A. Mohamed ◽  
Mohd. Imran ◽  
Monadil H. M. Ali ◽  
Mohammed F. Abdelwahab ◽  
Abdullrahman A. Alhaj
Keyword(s):  
Simultaneous Determination ◽  
Cost Effective ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Font Size ◽  
Chemometric Method ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Precision And Accuracy

<p style="margin: 0in 0in 0pt; text-align: justify; line-height: 150%;"><span style="line-height: 150%; font-family: 'Times New Roman','serif'; font-size: 12pt; mso-ascii-theme-font: major-bidi; mso-hansi-theme-font: major-bidi; mso-bidi-theme-font: major-bidi;">In the present study, a simple, inexpensive, precise and accurate uv-spectrophotometric method based on chemometrics, has been developed for the simultaneous determination of sulfadoxine and pyrimethamine in tablet formulation. The % recoveries obtained were 99.7% ± 0.9 and 101.5% ± 0.8 for sulfadoxine and pyrimethamine, respectively. The developed method has been compared to USP-HPLC method with regard to accuracy and precision. The calculated F-ratio and the (t) statistics indicate that there is no significant difference at 5% level with regard to precision and accuracy between the proposed and the USP methods. Moreover, the developed method is simple, cost-effective, and less time-consuming. Accordingly, it can be used advantageously in routine quality control of sulfadoxine and pyrimethamine in tablet formulation. </span></p>

Method for Trifuzol-Neo assay determination by GC-MS

2021 ◽  
pp. 4523-4528
Author(s):  
A.A. Yaroshenko ◽  
V.V. Parchenko ◽  
O.A. Bihdan ◽  
O.I. Panasenko ◽  
Yu V. Karpenko ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Quality Control ◽  
Mobile Phase ◽  
Raw Materials ◽  
Cost Effective ◽  
Scientific Interest ◽  
Research Information ◽  
Agricultural Chemistry ◽  
Derivatives Of

The derivatives of 1,2,4-triazole are of the great scientific interest in the fields of pharmaceutics, agricultural chemistry, and construction The production of Trifuzol-Neo has already been launched, and it is now commercially available. Compounds based on 1,2,4-triazole may also be useful in veterinary practice due to their antiviral activity. Trifuzol-Neo, or piperidinium ([5-(2-furanyl)-4-phenyl-4Н-1,2,4-triazol-3-yl]thio)acetate (Figure 1), has already proved to be an effective immunostimulator for poultry.Since that, the quality control of raw materials and the ready product is required during the production stage. Currently, there is only one method for determination of the assay of Trifuzol-Neo, which involves HPLC-DMD (Center of Medical Research Information and Patent and Licensing Practice of Ukraine. The main disadvantages of HPLC-DMD are the use of relatively high amounts of costly solvents (acetonitrile in this case), considerable baseline instability, and time-consuming system stabilization. Gas-chromatography is able to avoid these constrictions since it involves gas as a mobile phase, which is a more cost-effective and reproducible alternative. The newly developed GC/MS method for Trifuzol-Neo assay determination consists of the following steps: weighing 20.0mg of Trifuzol-Neo powder, dillution in 20mL methanol, injection of 0.5uL of the obtained solution to GC column (at least three times). The same operations are done with a Trifuzol-Neo standard.

HPTLC Method for the Determination of Metformin Hydrochloride, Saxagliptin Hydrochloride, and Dapagliflozin in Pharmaceuticals

2020 ◽  
Vol 16 (5) ◽  
pp. 609-619 ◽  
Author(s):  
Afnan E. Abdelrahman ◽  
Hadir M. Maher ◽  
Nourah Z. Alzoman
Keyword(s):  
Simultaneous Determination ◽  
High Specificity ◽  
Metformin Hydrochloride ◽  
Experimental Conditions ◽  
Pharmaceutical Tablets ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Hptlc Method

Background: Type 2 diabetes mellitus is an expanding health problem. Binary antidiabetic combinations of Metformin Hydrochloride (MET) with either Saxagliptin Hydrochloride (SAX), or Dapagliflozin (DAP) are widely used. Review of the literature revealed that no single HPTLC method has been reported for the simultaneous determination of MET, SAX, and DAP allowing the determination of binary mixtures of any two of the three cited drugs in their tablets using the same experimental conditions, an important advantage for quality control. The advantages of HPTLC method relies on the simultaneous analysis of a large number of samples in a shorter analysis time, less solvent consumption, and less expenses, compared with HPLC. Objective: The objective of the proposed method is to develop and validate a single and simple HPTLC densitometric method for the simultaneous determination of MET, SAX, and DAP. Methods: Separation was performed using aluminum HPTLC sheets coated with silica gel 60 F254 with a mobile phase consisting of a mixture of acetonitrile: 1% w/v ammonium acetate in methanol (9: 1, v/v). Scanning was performed at 210 nm. Results and Discussion: Linearity of the method was assessed in the concentration range of 0.25-10 μg/band for SAX and DAP and 0.25-25 μg/band for MET. The method was fully validated as per the ICH guidelines. The proposed method provided error and deviation values of less than 2% assessing good accuracy and precision. Conclusion: The method was successfully applied to the analysis of pharmaceutical tablets of MET/SAX, MET/DAP, and SAX/DAP with high specificity.

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