scholarly journals Development and application of a portable instrument for drugs analysis in pharmaceutical preparations

2015 ◽  
Vol 51 (3) ◽  
pp. 699-708
Author(s):  
Paulo Roberto da Silva Ribeiro ◽  
Helena Redigolo Pezza ◽  
Leonardo Pezza ◽  
Liliane Spazzapam Lima ◽  
Matthieu Tubino
Keyword(s):  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Ammonium Molybdate ◽  
Quantitative Studies ◽  
Significant Difference ◽  
Drugs Analysis ◽  
And Performance

This article describes the application and performance of an inexpensive, simple and portable device for colorimetric quantitative determination of drugs in pharmaceutical preparations. The sensor is a light detector resistor (LDR) incorporated into a black PTFE cell and coupled to a low-cost multimeter (Ohmmeter). Quantitative studies were performed with captopril/p-chloranil/H2O2 and methyldopa/ammonium molybdate systems. Calibration curves were obtained by plotting the electrical resistance of the LDR against the concentration of the colored species in the ranges 1.84 × 10-4 to 1.29 × 10-3mol L-1 and 5.04 × 10-4 to 2.52 × 10-3 mol L-1 for captopril/p-chloranil/H2O2 and methyldopa/ammonium molybdate systems, respectively, exhibiting good coefficients of determination. Statistical analysis of the results obtained showed no significant difference between the proposed methodologies and the official reported methods, as evidenced by the t-test and variance ratio at a 95% confidence level. The results of this study demonstrate the applicability of the instrument for simple, accurate, precise, fast,in situ and low-cost colorimetric analysis of drugs in pharmaceutical products.

Development and Validation of an Eco-Friendly and Low-Cost Method for the Quantification of Cefepime Hydrochloride in Powder for Injectable Solution Using Infrared (IR) Spectroscopy

2020 ◽  
Vol 16 (4) ◽  
pp. 456-464
Author(s):  
Danilo F. Rodrigues ◽  
Hérida R.N. Salgado
Keyword(s):  
Ir Spectroscopy ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Potassium Bromide ◽  
Pharmaceutical Products ◽  
Injectable Formulation ◽  
Ich Guidelines ◽  
Lactam Ring ◽  
Development And Validation

Background: A simple, eco-friendly and low-cost Infrared (IR) method was developed and validated for the analysis of Cefepime Hydrochloride (CEF) in injectable formulation. Different from some other methods, which employ organic solvents in the analyses, this technique does not use these types of solvents, removing large impacts on the environment and risks to operators. Objective: This study aimed at developing and validating a green analytical method using IR spectroscopy for the determination of CEF in pharmaceutical preparations. Methods: The method was validated according to ICH guidelines and the quantification of CEF was performed in the spectral region absorbed at 1815-1745 cm-1 (stretching of the carbonyl group of β- lactam ring). Results: The validated method showed to be linear (r = 0.9999) in the range of 0.2 to 0.6 mg/pellet of potassium bromide, as well as for the parameters of selectivity, precision, accuracy, robustness and Limits of Detection (LOD) and Quantification (LOQ), being able to quantify the CEF in pharmaceutical preparations. The CEF content obtained by the IR method was 103.86%. Conclusion: Thus, the method developed may be an alternative in the quality control of CEF sample in lyophilized powder for injectable solution, as it presented important characteristics in the determination of the pharmaceutical products, with low analysis time and a decrease in the generation of toxic wastes to the environment.

scholarly journals Spectrophotometric determination ofβ-blocker drugs by oxidation with bromate–bromide mixture and its analytical application to pharmaceutical preparations

2011 ◽  
Vol 25 (6) ◽  
pp. 303-315 ◽  
Author(s):  
Akram M. El-Didamony ◽  
Eman A. H. Erfan
Keyword(s):  
Indigo Carmine ◽  
Pharmaceutical Preparations ◽  
Reaction Conditions ◽  
Statistical Comparison ◽  
Spectrophotometric Methods ◽  
Significant Difference ◽  
Optimum Reaction ◽  
Comparison Of The Results

Three visible spectrophotometric methods (A–C) were developed for the analysis of someβ-blocker drugs, namely atenolol (ATE) and timolol (TIM) based on their reactivity with bromine, generated in situ by the action of hydrochloric acid on bromate–bromide mixture. The determination of residual bromine is based on its ability to bleach the indigo carmine dye and measuring the absorbance at 610 nm (method A). Methods B and C involve treating the unreacted bromine with a measured excess of iron (II), the remaining iron (II) is complexed with 1,10-phenanthroline (method B) or with 2,2'-bipyridyl (method C) and measuring the increase in absorbance at 510 and 522 nm, respectively. In all the methods, the amount of bromine reacted corresponding to the drug content. Regression analysis of Beer's plot showed good correlation in the concentration ranges of 0.4–16.4, 0.8–10.4 and 0.4–12.8 µg/ml using methods A–C, respectively, for ATE and 14–38, 12–32 and 14–38 µg/ml using methods A–C, respectively, for TIM. The optimum reaction conditions and other analytical parameters are evaluated. No interference was observed from the additives and the applicability of the methods was tested by analyzing the pharmaceutical preparations containing the investigated drugs. Statistical comparison of the results with those of official methods shows excellent agreement and indicates no significant difference in precision.

scholarly journals Influential Factors and Determination of strength of in-situ concrete, using twist-off method.

2019 ◽  
Vol 7 (2) ◽  
Author(s):  
Pooria Najarbashi ◽  
Mahmoud Naderi
Keyword(s):  
Low Cost ◽  
Concrete Strength ◽  
Influential Factors ◽  
Laboratory Methods ◽  
Significant Difference ◽  
Site Evaluation ◽  
In Situ Methods ◽  
Very High

Concrete strength represents by far the most critical property of concrete. It represents the mechanical properties of concrete. On-site evaluation of concrete strength remains the fundamental challenge in the condition assessment of existing infrastructure. Although standard laboratory methods can be typically used but most of these testing methods are costly and time-consuming. Among the in-situ methods, the “twist-off ” method with very slight damage is genuinely a convenient, fast and also low-cost technique that provides accurate results for engineers. In this study, the twist-offmethod has been used for the assessment of in-situ strength of the 30 concrete structures in Qazvin in Iran. The results showed structures studied had a strength of 45 to 600 kg/cm2 and the average is about 200 kg/cm2. The observed variation is very high, as well as a significant difference between the compressive strength of the columns, and the floors of the buildings that all indicate non-standard concrete mixing and inadequate control over construction. However, according to the past experience and results of the samples, some recommendations in this regard have been suggested.

scholarly journals Application of Thin-Layer Chromatography in Combination with Densitometry for the Determination of Diclofenac in Enteric Coated Tablets

2019 ◽  
Vol 12 (4) ◽  
pp. 183 ◽  
Author(s):  
Wioletta Parys ◽  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Degradation Products ◽  
Low Cost ◽  
Diclofenac Sodium ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Enteric Coated ◽  
Layer Chromatography

Diclofenac belongs to the drug class non-steroidal anti-inflammatory drugs widely used in Europe as well as all over the world. Thus, it is important to conduct research on its quality control of available pharmaceutical preparations like for example enteric coated tablets. Among various analytical techniques, thin-layer chromatography (TLC) is ideal for this task due to their short time analysis, ease of operation and low cost. Hence, the aim of this study was to develop the optimal conditions of analysis and quantitative determination of diclofenac sodium in enteric tablets by using TLC in combination with densitometry. Of all chromatographic systems tested, the best is the one which consists of silica gel 60F254 and cyclohexane: chloroform:methanol:glacial acetic acid (6:3:0.5:0.5 v/v) as the mobile phase, which allows the successful separation of examined diclofenac sodium as active component and the largest number (twelve) of its degradation products as potential impurities of its pharmaceutical products. This indicates that the newly developed method is more effective than previously reported assays by Starek and Krzek. Linearity range was found to be 4.00–18.00 μg/spot for diclofenac sodium. The results of the assay of enteric tablet formulations equals 98.8% of diclofenac sodium in relation to label claim is in a good agreement with pharmaceutical requirements.

scholarly journals Spectrophotometric determination of methyldopa in pharmaceutical formulations

2005 ◽  
Vol 30 (3) ◽  
pp. 23-28 ◽  
Author(s):  
P. R. S. Ribeiro ◽  
L. Pezza ◽  
H. R. Pezza
Keyword(s):  
Correlation Coefficient ◽  
Spectrophotometric Method ◽  
Confidence Level ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Products ◽  
Complexation Reaction ◽  
Excellent Correlation

A new, simple, precise, rapid and low-cost spectrophotometric method for methyldopa determination in pharmaceutical preparations is described. This method is based on the complexation reaction of methyldopa with molybdate. Absorbance of the resulting yellow coloured product is measured at 410 nm. Beer's Law is obeyed in a concentration range of 50 - 200 µg ml-1 methyldopa with an excellent correlation coefficient (r = 0.9999). No interference was observed from common excipients in formulations. The results show a simple, accurate, fast and readily applied method to the determination of methyldopa in pharmaceutical products. The analytical results obtained for these products by the proposed method are in agreement with those of the Brazilian Pharmacopoeia procedure at 95% confidence level.

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

scholarly journals A Simple, Rapid, Fluorometric Assay for Dopamine by In Situ Reaction of Boronic Acids and cis-Diol

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Xiaoxia Liu ◽  
Miaomiao Tian ◽  
Wenmei Gao ◽  
Jinzhong Zhao
Keyword(s):  
Low Cost ◽  
Boronic Acids ◽  
Emission Peak ◽  
Excitation Wavelength ◽  
Fluorescence Sensing ◽  
Serum Samples ◽  
Turn On ◽  
Rapid Reaction

An efficient, sensitive, and low-cost method has been developed for turn-on fluorescence sensing of dopamine (DA). The method relies on the rapid reaction of DA and 3-Hydroxyphenylboronic acid (3-HPBA) via specific recognition between boronic acids and cis-diol of DA in alkaline solution. The reaction product shows an excitation wavelength of 417 nm and the maximum emission peak at 470 nm. The proposed method allows the determination of DA in the range of 50 nM–25 μM, and the whole detection can be completed within 5 minutes. Furthermore, the presented approach has good selectivity and has been successfully applied to DA sensing in human serum samples, showing great potential in clinical diagnosis.

scholarly journals Simultaneous Determination of Sitagliptin and Metformin in Pharmaceutical Preparations by Capillary Zone Electrophoresis and its Application to Human Plasma Analysis

2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Capillary Zone Electrophoresis ◽  
Pharmaceutical Preparations ◽  
Effective Length ◽  
Relative Standard ◽  
Significant Difference ◽  
Zone Electrophoresis ◽  
Capillary Zone

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.

Fabrication of chemically and in situ modified carbon paste electrodes for the potentiometric determination of chlorpromazine HCl in pure pharmaceutical preparations, urine and serum

2017 ◽  
Vol 41 (24) ◽  
pp. 15612-15624 ◽  
Author(s):  
Gehad G. Mohamed ◽  
Eman Y. Z. Frag ◽  
M. A. Zayed ◽  
M. M. Omar ◽  
Sally E. A. Elashery
Keyword(s):  
Biological Fluids ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Carbon Paste ◽  
Chlorpromazine Hydrochloride ◽  
Carbon Paste Electrodes ◽  
Urine And Serum ◽  
Modified Carbon Paste Electrodes

Newly developed modified and in situ modified carbon paste sensors were developed for the determination of chlorpromazine hydrochloride (CPZHC) in pharmaceutical formulations and biological fluids (urine and serum).

Impact of Cytogenetic Abnormalities On Outcome Among Patients with Relapsed/Refractory Multiple Myeloma Treated with Bortezomib: Adverse Effect of 1q21 (CKS1B) Amplification.

Blood ◽  
2009 ◽  
Vol 114 (22) ◽  
pp. 2826-2826
Author(s):  
Hong Chang ◽  
Young Trieu ◽  
Connie Qi ◽  
Wei Xu ◽  
Donna E. Reece
Keyword(s):  
High Risk ◽  
Genetic Factors ◽  
Objective Response ◽  
Cytogenetic Abnormalities ◽  
Significant Difference ◽  
Variate Analysis ◽  
Ortho Biotech ◽  
Duration Of Response

Abstract Abstract 2826 Poster Board II-802 To investigate whether genetic risk factors affect the outcome of relapsed/refractory myeloma patients undergoing bortezomib therapy, we evaluated the clinical features of 85 patients treated with bortezomib and correlated with the high-risk cytogenetic abnormalities as detected by interphase cytoplasmic fluorescence in situ hybridization (cIg-FISH). Forty (47%) patients had an objective response to bortezomib with median progression free (PFS) and overall survivals (OS) of 9.4 and 12.6 months, respectively. cIg-FISH determination of del(13q), del(17p), del(1p21), t(4;14), and amp. (1q21)(CKS1B) was done on 79, 77, 77, 78, and 80 cases and the frequency of their detection was 38%, 22%, 26%, 18%, and 39%, respectively. There was no statistically significant difference in terms of response or duration of response to bortezomib for patients with or without any of the cytogenetic abnormalities. PFS was also comparable among patients with and without the aforementioned genetic markers. However, patients with 1q21(CKS1B) amplification had significantly shorter OS than those without such abnormality (5.3 vs. 24.6 months, p=0.0005). Multi-variate analysis adjusting for all 5 high-risk genetic factors confirmed that 1q21(CKS1B) amplification is an independent risk factor for OS (p=0.008). Improved therapeutic strategies may be required for this subgroup of patients. Disclosures: Reece: Ortho Biotech: Honoraria, Research Funding.

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