scholarly journals NON-DESTRUCTIVE RAMAN SPECTROSCOPIC METHOD FOR ESTIMATION OF MONTELUKAST FROM TABLET DOSAGES FORM

Author(s):  
Jwal Doctor ◽  
Palak Thakkar ◽  
Mitul Prajapati ◽  
Nrupresh Patel ◽  
Priti J. Mehta

Objective: A rapid, non-destructive and non-solvent raman spectroscopic method for estimation of Montelukast from tablet dosages form Methods: Quantification was carried out by measuring the intensity of analyte peak at 1440 cm-1. Each Raman spectrum corresponded to an accumulation of 4 scans with an exposure time of 5 sec for each scan with a total integration time of 20 sec.Results: The method exhibited linearity between 2 mg-24 mg show well resolve quantification From MON. The linearity equation was calculated as y = 13.036x+70.819 and the correlation coefficient was found to be 0.997 for MON. LOD (limit of detection) and LOQ(limit of quantification) values were calculated using the calibration curve slope and standard deviation of the response. The LOD (limit of detection) and LOQ (limit of quantification) values were found to be 1.71 mg and 5.13 mg respectively.Conclusion: The developed method was successfully applied for assay of montelukast in the intact formulation. The method was validated according to an international conference on harmonisation guidelines. A recent study, montelukast sodium had been analysed by the raman method, but, looking into the tremendous potential of raman spectroscopic method; it can be extended as a process analysis and technology tool in various quality checks during manufacturing of pharmaceutical products.

Processes ◽  
2020 ◽  
Vol 8 (7) ◽  
pp. 870
Author(s):  
Urszula Hubicka ◽  
Agnieszka Padiasek ◽  
Barbara Żuromska-Witek ◽  
Marek Szlósarczyk

Vitamin K is a group of lipophilic molecules. Forms of vitamin K play an essential role in the activation of specific proteins involved in blood clotting cascade or bone metabolism. Another molecule belonging to the fat-soluble vitamins group that also plays an important role in calcium metabolism is vitamin D3. The dietary supplements containing vitamins K and D3 are one of the most frequently consumed by patients. The objective of this work was to develop a simple, fast and sensitive thin-layer chromatography (TLC)-densitometric procedure for the simultaneous quantitative analysis of vitamins K and D3 in pharmaceutical products and dietary supplements. The analysis of vitamins was performed on the silica gel RP-18 F₂₅₄s plates with methanol-ethanol-isopropanol in a volume ratio of 15:1:4 as a mobile phase. The densitometric measurements were made at 254 nm. The method was validated by checking the specificity, linearity, precision, recovery, limit of detection, limit of quantification and robustness in accordance with International Conference on Harmonization (ICH) guidelines. The method was shown to be specific, accurate (recoveries were from 95.78 to 104.96%), linear over the tested range (correlation coefficient, exceeding 0.99), and precise (precision and intermediate precision RSD below 2.70% for all analytes). The satisfactory results of the validation of the method indicate that it can be used in the quality control of dietary supplements and pharmaceutical products containing vitamins K and D3.


Author(s):  
Dhanya B. Sen ◽  
Ashim K. Sen ◽  
Aarti S. Zanwar ◽  
Harshita Pandey ◽  
Rajesh A. Maheshwari

Three new, precise, accurate and sensitive UV-Spectrophotometric methods namely Ratio Difference Spectroscopic Method (RDSM), First Derivative of Ratio Spectra Method (DR1) and Area Under Curve Method (AUC) were developed and validated for simultaneous assessment of alogliptin benzoate (ALO) and pioglitazone hydrochloride (PIO) in tablet dosage form. In RDSM, ratio spectra of both the drugs were recorded by dividing the mixtures using interfering drug as divisor. Then the difference between the amplitudes of obtained ratio spectra was measured at 288 and 291 nm for ALO and 236 and 245 nm for PIO. The second method DR1, where the first derivative of ratio spectra of both the drugs were recorded and the first derivative signal was measured at 290 nm for ALO and 276.8 nm for PIO. The scaling factor was fixed as 1 and wavelength interval (Δλ) as 2 for recording the first derivative of ratio spectra.  In the third method (AUC), peak area of recorded zero order spectra was measured at 276 ± 10 nm for ALO and 267.8 ± 10 nm for PIO. All three proposed methods were validated according to “International Conference on Harmonization” (ICH) guidelines parameters. For all three methods, ALO and PIO obeyed Beer’s law in the range of 0.5-5 & 1.8-18 µg/ml, respectively. The % RSD of repeatability of measurement, intra-day and inter-day precision were found to be less than 2 for all three methods. Limit of detection (LOD) and Limit of quantification (LOQ) of the drugs were calculated which proved the sensitivity of the methods. The accuracy ranged between 98-101% for all three methods. No interference from pharmaceutical excipients present in the formulation was observed.  These proposed methods were found to be simple, sensitive, accurate and precise and can be applied to the simultaneous estimation of ALO and PIO in combined tablet formulation and also appropriate for routine quality control analysis.


Inventions ◽  
2021 ◽  
Vol 6 (3) ◽  
pp. 57
Author(s):  
Ramona Oana Gunache (Roșca) ◽  
Alexandra Virginia Bounegru ◽  
Constantin Apetrei

This paper presents an accurate and fast electrochemical method for atorvastatin determination in pharmaceutical products. Two screen-printed sensors, one—carbon based (SPCE) and one based on carbon nanotubes and gold nanoparticles (AuNP-CNT/SPCE) were used during the electrochemical analyses. At all experimental stages, cyclic voltammetry was employed, both for the characterization of the sensors and their electrochemical behavior, and for quantitative determinations. AuNP-CNT/SPCE has showed an extended active area, higher intensity peaks, better reversibility and lower background current than the unmodified sensor. For atorvastatin quantification, a calibration curve has been developed within the 1.2–606.25 µM concentration range. A linearity relation between the current of the anodic peak and concentration has been obtained in the range 1.2–53.33 µMfor both sensors. With the AuNP-CNT/SPCE sensor, low values of limit of detection, LOD (1.92 × 10−7 M) and limit of quantification, LOQ (6.39 × 10−7 M) have been obtained, which demonstrates the feasibility of the method of determining atorvastatin from real samples. Atorvastatin amount has been successfully determined from pharmaceutical products using AuNP-CNT/SPCE. The results were similar to the manufacturer’s specifications regarding the dosage per tablet and to the concentrations obtained by applying the FTIR spectrometric method.


2021 ◽  
Vol 22 (1) ◽  
pp. 115-126
Author(s):  
Zahid Ali Zounr

An easy, sensitive and accurate spectrophotometric method has been developed for the determination of Lisinopril (LNP) in pure and tablet formulations based on derivatization reaction with 2-hydroxynaphthaldehyde (2HNA). The derivatization reaction was carried out in methanol solvent at pH-5.5 at 95±2C for 15 min. The linear calibration curve was obtained that obeyed the Beer’s law within the concentration range 5-50 μgmL-1 of LNP at 433 nm with a coefficient of determination R²=0.996. The recovery was in the range from 98.25-101.82 with molar absorptivity of drug 9×103 mole-1cm-1. The method was accurate and precise (intra-day variation 0.05-0.97% and inter-day 0.07-1.6%), with limit of detection (LOD) and limit of quantification (LOQ) 0.264 μgmL-1 and 0.8 μgmL-1, respectively. No interferences from the excipients were detected. The method was applied for the rapid analysis of LNP in pharmaceutical products.


2018 ◽  
pp. 13
Author(s):  
Santi Maha Dewi

Solvent extracted results are often not utilized for re-extraction. Methanol is a universal solvent which is often used as an extract of simplicia. The result of a rotary vacuum evaporator distillation is not known purity and level. Raman spectrosphotometer is a non destructive method of analysis that can be applied to determine the levels and purity of distilled methanol. The objective of this research is to know the change of vacuum pressure to the level and purity of methanol, so that methanol from rotary vacuum distillation can be reused for re-extraction. Purple sweet potato leaves are macerated using 95% methanol : 3% citric acid. The extract was evaporated using a rotary vacuum evaporator at 100 mbar, 150 mbar, and 200 mbar vacuum pressure with a range of 5 to 180 min. Purity and methanol levels were determined using a Raman Handheld 1064 nm spectrophotometer. Validation of methanol assay method with Raman spectrophotometer was obtained: precision: KV 0.19% -1.70%, accuracy: 94.4-103.8%, limit of detection: 1.77% (v/v), limit of quantification: 5.89% (v/v), the range of linearity of 1.77% -99.9% (v/v), with a calibration curve equation: y = 216,88x + 1437.1 and the value of R2 = 0.9997. Methanol content of distillation product with pressure variation 100 - 200 mbar in the span of 5 to 180 minutes obtained methanol level 59.8-81.2% (v/v). All distilled methanol yields a spectrum similarity of 86-99% when compared with absolute methanol.


2015 ◽  
Vol 51 (4) ◽  
pp. 879-891 ◽  
Author(s):  
Serpil Sevim ◽  
Nevin Erk

abstract The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC) and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4) and acetonitrile (35:65 by volume). The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL) and limit of quantification (50 ng/mL) were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000). In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method.


2012 ◽  
Vol 7 (10) ◽  
pp. 1934578X1200701
Author(s):  
Bojidarka Ivanova ◽  
Michael Spiteller

This paper reports the qualitative and quantitative analysis (QA) of mixtures of hallucinogens, N,N-dimethyltryptamine (DMT) (1), 5-methoxy- (1a) and 5-hydroxy- N,N-dimethyltryptamine (1b) in the presence of β-carbolines (indole alkaloids of type XII) {(2), (3) and (5)}. The validated electronic absorption spectroscopic (EAs) protocol achieved a concentration limit of detection (LOD) of 7.2.10-7 mol/L {concentration limit of quantification (LOQ) of 24.10-7mol/L} using bands (λmax) within 260±0.23-262±0.33 nm. Metrology, including accuracy, measurement repeatability, measurement precision, trueness of measurement,and reproducibility of the measurements are presented using N,N- dimethyltryptamine (DMA) as standard. The analytical quantities of mixtures of alkaloids 4, 6 and 7 are: λmax 317±0.45, 338±0.69 and 430±0.09 for 4 (LOD, 8.6.10-7 mol/L; LOQ, 28.666, mol/L), as well as 528±0.75 nm for 6 and 7 (LOD, 8.2. 10-7 mol/L; LOQ, 27.333, mol/L), respectively. The partially validated protocols by high performance liquid chromatography (HPLC), electrospray ionization (ESI), mass spectrometry (MS), both in single and tandem operation (MS/MS) mode, as well as matrix/assisted laser desorption/ionization (MALDI) MS are elaborated. The Raman spectroscopic (RS) protocol for analysis of psychoactive substances, characterized by strong fluorescence RS profile was developed, with the detection limits being discussed. The known synergistic effect leading to increase the psychoactive and hallucinogenic properties and the reported acute poisoning cases from 1-7, make the present study emergent, since as well the current lack of analytical data and the herein metrology obtained contributed to the elaboration of highly selective and precise analytical protocols, which would be of interest in the field of criminal forensic analysis.


Nanomaterials ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 1266
Author(s):  
Aftab A. Khand ◽  
Saeed A. Lakho ◽  
Aneela Tahira ◽  
Mohd Ubaidullah ◽  
Asma A. Alothman ◽  
...  

Recently, the oxidative behavior of methotrexate (MTX) anticancer drug is highly demanded, due to its side effects on healthy cells, despite being a very challenging task. In this study, we have prepared porous NiO material using sodium sulfate as an electronic disorder reagent by hydrothermal method and found it highly sensitive and selective for the oxidation of MTX. The synthesized NiO nanostructures were characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) techniques. These physical characterizations delineated the porous morphology and cubic crystalline phase of NiO. Different electrochemical approaches have been utilized to determine the MTX concentrations in 0.04 M Britton–Robinson buffer (BRB) at pH 2 using glassy carbon electrode (GCE)-modified with electronically disordered NiO nanostructures. The linear range for MTX using cyclic voltammetry (CV) was found to be from 5 to 30 nM, and the limit of detection (LOD) and limit of quantification (LOQ) were 1.46 nM and 4.86 nM, respectively, whereas the linear range obtained via linear sweep voltammetry (LSV) was estimated as 15–90 nM with LOD and LOQ of 0.819 nM and 2.713 nM, respectively. Additionally, amperometric studies revealed a linear range from 10 to70 nM with LOD and LOQ of 0.1 nM and 1.3 nM, respectively. Importantly, MTX was successfully monitored in pharmaceutical products using the standard recovery method. Thus, the proposed approach for the synthesis of active metal oxide materials could be sued for the determination of other anticancer drugs in real samples and other biomedical applications.


The Analyst ◽  
2018 ◽  
Vol 143 (18) ◽  
pp. 4347-4353
Author(s):  
Donghyun Ryoo ◽  
Jong Yun Kim ◽  
Pham Khac Duy ◽  
Sang Hoon Cho ◽  
Hoeil Chung ◽  
...  

A versatile Raman spectroscopic method to determine the contents of carbon nanotubes (CNTs) in CNT/polydimethylsiloxane (PDMS) composites is demonstrated, and important issues directly related to the accuracy of the measurement were investigated.


1970 ◽  
Vol 3 (1) ◽  
pp. 4-10
Author(s):  
Kanij Fatema ◽  
Md Zakiur Rahman ◽  
Subrata Kumar Biswas ◽  
Suraia Akter

Nefopam and Escitalopram are INN drugs and as such it has not been yet included in the BP or USP. The objective of this work is to develop a simple, sensitive, accurate, precise and reproducible UVSpectrophotometric method for quantitative estimation of Nefopam and Escitalopram in tablet dosage forms. Various solvents were used to find out the medium for maximum solubility of each drug. The χmax of Nefopam and Escitalopram was 266nm and 284nm in water respectively. Both drugs obey Beer- Lambert’s law in the range of 50-400μg/ml for Nefopam and 25-200μg/ml for Escitalopram. The correlation coefficients of std. curves were 0.998 and 0.995. The values of SD were 0.131 and 0.081 respectively. %RSD (Relative standard deviation) of interday absorbance of Nefopam was 0.766 and Escitalopram was 0.854. The LOD (Limit of Detection) were 0.393 and 0.243 and LOQ (Limit of Quantification) were 1.310 and 0.810 respectively. The percent potencies were 92.16 and 102.06 for Nefopam and Escitalopram. The potency of these tablets complied with their claimed quantity (±10%). So, based on these data, it may be concluded that these proposed method are simple, sensitive, precise, reproducible and accurate for the analysis of these drugs in tablet dosage form. Key Words: INN drugs; correlation coefficients; LOD; LOQ; Nefopam; Escitalopram. DOI: 10.3329/sjps.v3i1.6791S. J. Pharm. Sci. 3(1): 4-10


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