VALIDATED NOVEL SPECTROSCOPIC METHOD FOR ESTIMATION OF TRIAMCINOLONE ACETONIDE IN NASAL SPRAY

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (10) ◽  
pp. 51-55
Author(s):  
Satish A. Patel ◽  
Bhoomi H. Patel ◽  
Keyword(s):  
Triamcinolone Acetonide ◽  
Nasal Spray ◽  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Cost Effective ◽  
Isosbestic Point ◽  
Limit Of Quantification ◽  
Nasal Sprays ◽  
Ich Guideline

A simple, sensitive, accurate, precise and cost-effective pH independent spectrophotometric method has been developed for the estimation of triamcinolone acetonide in nasal sprays. Estimation was carried out at the isosbestic point of drug solutions, Isosbestic point was measured by scanning equimolar solution of triamcinolone acetonide separately in phosphate buffer pH 3.0, phosphate buffer pH 7.0 and phosphate buffer pH 10.0 at a concentration of 10 µg mL-1. They were scanned in the wavelength range of 200-400 nm. The isosbestic point was found to be 230.0 nm in acidic, basic and neutral condition; hence pH independent wavelength 230 nm was used for estimation of triamcinolone acetonide. The method observed linear response in the concentration range of 3-18 µg mL-1 at 230 nm. Developed method has been validated in accordance with ICH guideline Q2 R1 for several parameters like linearity, precision, accuracy, limit of detection and limit of quantification. The developed and validated analytical method was successfully applied to the estimation of triamcinolone acetonide in marketed nasal spray formulations.

scholarly journals UPLC Method Optimisation and Validation for the Estimation of Sodium Cromoglycate in Pressurized Metered Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 18-24
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Sodium Cromoglycate ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Calibration Graph ◽  
Assay Method ◽  
Dose Inhaler ◽  
Limit Of Quantification ◽  
Adequate Accuracy ◽  
Metered Dose ◽  
Ich Guideline

UPLC assay method optimised and validated for sodium cromoglycate in metered dose inhaler (MDI) using metronidazoleas an internal standard.The separation of Sodium Cromoglycate was achieved on Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) with gradient mobile phase containing methanol, orthophosphoric acid and acetonitrile in the ratio of 50:15:35 %v/v/v. The flow rate was 0.25 mLmin-1, injection volume 20μl and detection wavelength was set at 326nm, at ambient temperature. The validation of the proposed method was carried outfor linearity, accuracy, precision, robustness, limit of detection and limit of quantification test as per ICH guideline. The retention time of sodium cromoglycate found to be 4.73 min. Calibration graph was found to be linear at range 8- 40μg/ml. The regression coefficient (r2) was found tobe 0.9978.The proposed method was rapid with adequate accuracy, precision, ruggedness and robustness and hence be suitable for theroutine analysis of sodium cromoglycate in meter dose inhalation and in bulk.

scholarly journals Development of the UV Spectrophotometric Method of Azithromycin in API and Stress Degradation Studies

2016 ◽  
Vol 68 ◽  
pp. 48-53 ◽  
Author(s):  
Sandip Bhimani ◽  
Gaurav Sanghvi ◽  
Trupesh Pethani ◽  
Gaurav Dave ◽  
Vishal Airao ◽  
...  
Keyword(s):  
Linear Relationship ◽  
Spectrophotometric Method ◽  
Phosphate Buffer ◽  
Macrolide Antibiotic ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Limit Of Quantification ◽  
Absorbance Maximum ◽  
Antibiotic Drug ◽  
Stress Degradation

Azithromycin (AZI) is a semi-synthetic macrolide antibiotic drug, effective against a wide variety of bacteria. The present study describes a simple, accurate, reproducible and precise UV Spectrophotometric method for the estimation of AZI (pH 6.8 Phosphate buffer). The absorbance maximum (λmax) for AZI was found to be 208nm. The method reveals high sensitivity, with linearity in the 10 µg/ml to 50 µg/ml range. The lower limit of detection was found to be 1.6µg/ml and the limit of quantification was found to be 5µg/ml. All the calibration curves demonstrated a linear relationship between the absorbance and concentration, with the correlation coefficient higher than 0.99. The % recovery was found to be 99.72%. AZI was also subjected to stress degradation under different conditions recommended by the International Conference on Harmonization (ICH).

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

2017 ◽  
Vol 9 (6) ◽  
pp. 161
Author(s):  
Jwal Doctor ◽  
Palak Thakkar ◽  
Mitul Prajapati ◽  
Nrupresh Patel ◽  
Priti J. Mehta
Keyword(s):  
Limit Of Detection ◽  
Process Analysis ◽  
Spectroscopic Method ◽  
Pharmaceutical Products ◽  
Integration Time ◽  
Limit Of Quantification ◽  
Raman Spectroscopic ◽  
Quality Checks ◽  
Technology Tool ◽  
Non Destructive

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.

Novel HILIC-ESI-MS method for urinary profiling of MSUD and methylmalonic aciduria biomarkers

2019 ◽  
Vol 57 (8) ◽  
pp. 715-723
Author(s):  
Elizabeth Mary Mathew ◽  
Leslie Lewis ◽  
Pragna Rao ◽  
K Nalini ◽  
Asha Kamath ◽  
...  
Keyword(s):  
Formic Acid ◽  
Malonic Acid ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Methylmalonic Aciduria ◽  
Limit Of Quantification ◽  
Maple Syrup ◽  
Effective Manner ◽  
Branched Chain ◽  
Development And Validation

AbstractMethyl malonic acid and branched-chain keto acids are important biomarkers for the diagnosis of cobalamin deficiencies and maple syrup urine disease. We report the development and validation of a HILIC-ESI-MS2 method for the quantification of these organic acids from neonatal urine. The samples were 100 times diluted and analyzed on a ZIC-HILIC column with 25-mM formic acid in water: 25-mM formic acid in acetonitrile (45:55) at a flow rate of 0.8 mL/min with a runtime of only 6 minutes. The method demonstrated a lower limit of detection of 10 ng/mL, Limit of Quantification (LOQ) of 50 ng/mL, linearity of r2 ≥ 0.990 and recoveries of 87–105% for all analytes. The intraday and interday precision CV’s were <10% and 12%, respectively. Extensive stability studies demonstrated the analytes to be stable in stock and in matrix with a percent change within ±15%. The Bland–Altman analysis of the developed method with the gold standard GCMS method demonstrated a bias of 0.44, 0.11, 0.009 and –0.19 for methyl malonic acid, 3-methyl-2-oxovaleric acid, 2-hydroxy-3methylbutyric acid and 4-methyl-2-oxovaleric acid, respectively, proving the methods are comparable. The newly developed method involves no derivatization and has a simple sample preparation and a low runtime, enabling it to be easily automated with a high sample throughput in a cost-effective manner.

scholarly journals Visualization of Aspalathin in Rooibos (Aspalathus linearis) Plant and Herbal Tea Extracts Using Thin-Layer Chromatography

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 938 ◽  
Author(s):  
Emily Amor Stander ◽  
Wesley Williams ◽  
Fanie Rautenbach ◽  
Marilize Le Roes-Hill ◽  
Yamkela Mgwatyu ◽  
...  
Keyword(s):  
Quality Control ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Throughput Screening ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Herbal Tea ◽  
Limit Of Quantification ◽  
Aspalathus Linearis ◽  
Layer Chromatography

Aspalathin, the main polyphenol of rooibos (Aspalathus linearis), is associated with diverse health promoting properties of the tea. During fermentation, aspalathin is oxidized and concentrations are significantly reduced. Standardized methods for quality control of rooibos products do not investigate aspalathin, since current techniques of aspalathin detection require expensive equipment and expertise. Here, we describe a simple and fast thin-layer chromatography (TLC) method that can reproducibly visualize aspalathin in rooibos herbal tea and plant extracts at a limit of detection (LOD) equal to 178.7 ng and a limit of quantification (LOQ) equal to 541.6 ng. Aspalathin is a rare compound, so far only found in A. linearis and its (rare) sister species A. pendula. Therefore, aspalathin could serve as a marker compound for authentication and quality control of rooibos products, and the described TLC method represents a cost-effective approach for high-throughput screening of plant and herbal tea extracts.

scholarly journals Development and ICH Validation of a RP-HPLC-UV Method for the Quantification of Thimerosal in Topic Creams

2017 ◽  
Vol 60 (4) ◽  
Author(s):  
Guadalupe Pérez-Caballero ◽  
Nancy Muro-Hidalgo ◽  
Elvia Adriana Morales-Hipólito ◽  
Alma Villaseñor ◽  
Raquel López-Arellano
Keyword(s):  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Reversed Phase ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Quality Control Tool

A reversed phase high-performance liquid chromatography (RP-HPLC) method for determination of Thimerosal (TMS) in topical creams was optimized and validated according to the ICH guidelines which include accuracy, precision, selectivity, robustness, limit of detection (LOD), limit of quantification (LOQ), linearity and range. For topical creams, sample treatment is often an overwhelming step essentially due to its oily nature. For the first time a simple and robust extraction procedure for TMS using phosphate buffer (pH 5.5, 0.2M) was successfully developed. This method describes the TMS quantitation by HPLC in a topical product containing 0.01% fluocinolone acetonide (FLA) as the active molecule. The HPLC separation was achieved on a Column Symmetry® and a methanol: phosphate buffer (pH 2.5, 0.05M) 70:30 v/v mobile phase and wavelength 218 nm. Results from both standards and samples showed adequate validation parameters. Noteworthy, linearity was within the range 1.2 - 2.8 μg/mL. Additionally, robustness and TMS stability were established after sample extraction. The method provides an efficient and safe quality control tool for determination of TMS in topical creams.

scholarly journals A Simple and Cost-Effective TLC-Densitometric Method for the Quantitative Determination of Acetylsalicylic Acid and Ascorbic Acid in Combined Effervescent Tablets

Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3115 ◽  
Author(s):  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy ◽  
Wioletta Parys ◽  
Katarzyna Bober ◽  
Grażyna Janikowska
Keyword(s):  
Ascorbic Acid ◽  
Quantitative Determination ◽  
Acetylsalicylic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Volume Ratio ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification

A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50–9.00 μg/spot and 1.50–13.50 μg/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.

scholarly journals UV Spectrophotometric Methods to Quantify Alogliptin Benzoate and Pioglitazone Hydrochloride

2021 ◽  
pp. 31-41
Author(s):  
Dhanya B. Sen ◽  
Ashim K. Sen ◽  
Aarti S. Zanwar ◽  
Harshita Pandey ◽  
Rajesh A. Maheshwari
Keyword(s):  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ich Guidelines ◽  
The Difference ◽  
Tablet Dosage

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.

scholarly journals Quantitative determination of cyanoacetic acid content in teriflunomide drug substance by ion chromatography using conductivity detector

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Kishore V. Merusomayajula ◽  
T. Siva Rao ◽  
K. Rama Srinivas ◽  
Ch. V. Sathyendranath
Keyword(s):  
Ion Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Drug Substance ◽  
Cyanoacetic Acid ◽  
Limit Of Quantification ◽  
Elution Time ◽  
Suppressed Conductivity Detection

Abstract Background The current study focuses on the development and validation of an analytical method for quantifying cyanoacetic acid (CAA) in teriflunomide drug substance using a high-performance ion chromatography (IC) with cation suppressed conductivity detection (TFM). Water was used as the diluent for preparing the sample solution, which was injected into a standard chromatographic device with 250 mm, 4.0 mm ID, and 5.0 μm particle size Metrosep A Supp 5 Ion exchange column and a suppressed conductivity detector. At a flow rate of 0.6 mL min−1 and a temperature of 40 °C, the mobile phase was delivered in an isocratic mode. Results CAA and TFM had retention times of 12.78 and 15.82 min, respectively. CAA has a limit of detection (LOD) of 33 μg/g and a limit of quantification (LOQ) of 101 μg/g, respectively. For LOD and LOQ accuracy, the percentage RSD of CAA is 1.7 and 1.2, respectively. The average CAA recovery percentage was found to be between 98.6 and 100.1%. With a value of 0.9998, the calibration curve yielded an excellent linear correlation coefficient for CAA. According to the ICH guidelines, all verification parameters are within the range, indicating that the system is stable. Conclusion The elution time and run time in the currently developed ion chromatography analytical method have been reduced, demonstrating that the method is cost-effective and generally accepted, as well as simple and functional, and can be used in routine quality control tests in the industry.

Development and Validation of UV-Spectrophotometric Methods for the Determination of Berberine in Polymeric Nanoparticles

2019 ◽  
Vol 11 (12) ◽  
pp. 1273-1278
Author(s):  
Md Ali Mujtaba
Keyword(s):  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Polymeric Nanoparticles ◽  
Uv Spectroscopy ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Development And Validation

A simple, specific, economic, accurate, and reproducible UV-spectrophotometric methods were developed and validated for the estimation of berberine (BRC) in bulk and pharmaceutical formulation. The λmax of BRC in 0.1 N hydrochloric acid (pH 1.2), phosphate buffer (pH 6.8), and water was found to be 346 nm, 343 nm and 260 nm respectively. Beer's law was obeyed in the concentration range of 5–30 μg/ml (R2 = 0.9698) in water, 5–25 μg/ml (R2 = 0.9991) in 0.1 N HCl buffer (pH 1.2) and 5–35 μg/ml (R2 = 0.9935) in phosphate buffer (pH 6.8). These methods were tested, and validated for various parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD), and limit of quantification (LOQ) according to ICH guidelines. The method showed good reproducibility and recovery with percent relative standard deviation less than 2%. Moreover, the accuracy and precision obtained implied that UV spectroscopy can be a cheap, reliable, and less time consuming alternative for chromatographic analysis. The proposed methods were successfully applied for the determination of BRC in pharmaceutical formulation. The BRC estimated from the formulation was found to be well within limits (±5% of the labelled content of the formulations). The proposed methods are highly sensitive, precise, accurate, and can be employed for the routine analysis of berberine in bulks as well as in the commercial formulations.

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