scholarly journals Determination of Vitamins K1, K2 MK-4, MK-7, MK-9 and D3 in Pharmaceutical Products and Dietary Supplements by TLC-Densitometry

Processes ◽  
2020 ◽  
Vol 8 (7) ◽  
pp. 870
Author(s):  
Urszula Hubicka ◽  
Agnieszka Padiasek ◽  
Barbara Żuromska-Witek ◽  
Marek Szlósarczyk
Keyword(s):  
Dietary Supplements ◽  
Vitamin K ◽  
Limit Of Detection ◽  
Volume Ratio ◽  
Pharmaceutical Products ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Clotting Cascade ◽  
Fat Soluble Vitamins ◽  
Analysis Of Vitamins

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.

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.

scholarly journals Determination of Synephrine in Bitter Orange Raw Materials, Extracts, and Dietary Supplements by Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation

2007 ◽  
Vol 90 (1) ◽  
pp. 68-81 ◽  
Author(s):  
Mark C Roman ◽  
Joseph M Betz ◽  
Jana Hildreth
Keyword(s):  
Dietary Supplements ◽  
Biogenic Amine ◽  
Limit Of Detection ◽  
Raw Materials ◽  
Raw Material ◽  
Limit Of Quantification ◽  
Bitter Orange ◽  
Amine Content ◽  
Minor Compounds ◽  
Single Laboratory

Abstract A method has been developed to quantify synephrine in bitter orange raw material, extracts, and dietary supplements. Single-laboratory validation has been performed on the method to determine the repeatability, accuracy, selectivity, limit of detection/limit of quantification (LOQ), ruggedness, and linearity for p-synephrine and 5 other biogenic amines: octopamine, phenylephrine (m-synephrine), tyramine, N-methyltyramine, and hordenine, which may be present in bitter orange. p-Synephrine was found to be the primary biogenic amine present in all materials tested, accounting for >80 of the total biogenic amine content in all samples except a finished product. Repeatability precision for synephrine was between 1.48 and 3.55 RSD. Synephrine recovery was between 97.5 and 104. The minor alkaloids were typically near the LOQ of the method (300900 g/g) in the test materials, and between-day precision for the minor compounds was poor because interferences could sometimes be mistakenly identified as one of the minor analytes. Recoveries of the minor components ranged from 99.1 to 103 at approximately 6000 g/g spike level, to 90.7 to 120 at 300 g/g spike level.

scholarly journals Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

scholarly journals Determination of crinamidine in dietary supplements by GC-MS/MS

2018 ◽  
Vol 1 (1) ◽  
pp. 3-7
Author(s):  
Lien Le Thi ◽  
Anh Bach Thuy ◽  
Khanh Cao Cong ◽  
Ha Tran Nguyen ◽  
Hong Hao Le Thi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Calibration Curve ◽  
Limit Of Detection ◽  
Coefficient Of Determination ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Precision Limit

The determination of crinamidine in dietary supplements content by mass spectrometry (GC-MS/MS) was developed and validated. The method was performed on the DB5MS column (30m x 0,25mm; 0,25 μm), in combination with the tandem mass spectrometry. The parameters of the method were evaluated for selectivity, calibration curve, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination 0.9970) within the concentration range of 5ppm-50ppm. The recovery at three concentrations were above 90,1%. The limit of detection (LOD) and limit of quantification (LOQ) of the methods were 3 and 10 mg/kg, respectively. All obtained results were acceptable according to the AOAC for dietary supplements. The method was applied to analyze 34 samples in Hanoi.

scholarly journals STABILITY INDICATING VALIDATED HPLC METHOD FOR THE DETERMINATION OF ZANUBRUTINIB IN BULK AND PHARMACEUTICAL DOSAGE FORM

2020 ◽  
pp. 159-162
Author(s):  
M. VIJAYA KUMARI ◽  
CH. BALASEKHAR REDDY
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Acceptable Limit ◽  
Relative Standard

Objective: An accurate, rapid economical and straight forward, reliable assay technique was evolved and showed for the evaluation of zanubrutinib using reversed-phase high-performance liquid chromatography. Methods: In the proposed method, efficient chromatographic separation was achieved applying acetonitrile and 0.1% orthophosphoric acid (50:50 v/v) as a mobile phase with a flow of 1 ml/min and the wavelength was observed at 220 nm. Chromatography was administered isocratically at ambient temperature and run time was approximately 6 min and the retention time (Rt) was observed as 4.358 min. Results: The method was justified as per ICH guidelines. System suitability parameters were studied by injecting the quality six fold and results were well under acceptance criteria. Linearity study was administered between 10% and 150% levels, regression coefficient value was observed as 0.999. Limit of detection and limit of quantification were observed as 0.02 μg/ml and 0.2 μg/ml, respectively. Precision was found to be 0.74 for repeatability and 0.68 for intermediate precision. Recovery of the drug was found to be 98–102%, indicates that the recovery is in the acceptable limit. Validation results were found to be satisfactory and the method applicable for bulk and formulation analysis. Hence, it was evident that the proposed method was said to be suitable for regular analysis and quality control of pharmaceutical preparations. Conclusion: The validation results were in good agreement with the acceptable limit. Relative standard deviation values which are <2.0% indicating the accuracy and precision of this method. Assay of retail formulation was administered and found to be 100.24% was present using the above method. Stress conditions of degradation in acidic, alkaline, peroxide, and thermal were studied. This developed method showed reliable, precise, accurate results under optimized conditions.

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 HPTLC Method for Simultaneous Determination of Lopinavir and Ritonavir in Capsule Dosage Form

2008 ◽  
Vol 5 (4) ◽  
pp. 706-712 ◽  
Author(s):  
A. V. Sulebhavikar ◽  
U. D. Pawar ◽  
K. V. Mangoankar ◽  
N. D. Prabhu-Navelkar
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Uv Light ◽  
Pharmaceutical Preparation ◽  
Volume Ratio ◽  
Detector Response ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Hptlc Method

A rapid and simple high performance thin layer chromatography (HPTLC) method with densitometry at λ=263 nm was developed and validated for simultaneous determination of lopinavir and ritonavir from pharmaceutical preparation. Separation was performed on aluminum-backed silica gel 60F254HPTLC plates as stationary phase and using a mobile phase comprising of toluene, ethyl acetate, methanol and glacial acetic acid, in the volume ratio of 7.0:2.0:0.5:0.5 (v/v) respectively. After development, plates were observed under UV light. The detector response was linear in the range of 6.67 to 20.00 µg/spot and 1.67 to 5.00 µg/spot for lopinavir and ritonavir respectively. The validated lowest limit of detection was 21.00 ng/spot and 5.10 ng/spot whereas lowest limit of quantification was 7.00 ng/spot and 21.00 ng/spot for lopinavir and ritonavir respectively. The percentage assay of lopinavir and ritonavir was found between 98.23 to 102.28% and 98.03 to 103.50% respectively. The described method has the advantage of being rapid and easy. Hence it can be applied for routine quality control analysis of lopinavir and ritonavir from pharmaceutical preparation and stability studies.

scholarly journals Development of the simultaneous analysis of choline salicylate, lidocaine hydrochloride and preservatives in a new dental gel by HPLC method

Chemija ◽  
2021 ◽  
Vol 32 (2) ◽  
Author(s):  
Yuliia Maslii ◽  
Ivan Bezruk ◽  
Anna Materiienko ◽  
Olena Ruban ◽  
Liudas Ivanauskas ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Hplc Method ◽  
Lidocaine Hydrochloride ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Intermediate Precision

A new high-performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of active pharmaceutical substances and preservatives in a new dental medication has been developed. The optimization of HPLC method parameters was done through studies of a mobile phase composition and a detection wavelength. Our developing method uses an ACE C18 column (250 × 4.6 mm, 5 µm) and a gradient mode for separation with the acetonitrile and phosphate buffer solution (adjusted to pH 3.0) as mobile phases. The flow rate is 1 ml/ min, and the detection was set at 260 nm (DAD). The method was evaluated according to the ICH guidelines and the State Pharmacopoeia of Ukraine in terms of specificity, accuracy, linearity and precision (repeatability and intermediate precision). The limit of detection and the limit of quantification were also calculated. The developed method was put in place for the analysis of a combined dental gel to a quantitative determination of the APIs (choline salicylate, lidocaine hydrochloride) and preservatives (methylparaben, propylparaben).

scholarly journals Determination of Atorvastatin with Voltammetric Sensors Based on Nanomaterials

Inventions ◽  
2021 ◽  
Vol 6 (3) ◽  
pp. 57
Author(s):  
Ramona Oana Gunache (Roșca) ◽  
Alexandra Virginia Bounegru ◽  
Constantin Apetrei
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Products ◽  
Spectrometric Method ◽  
Background Current ◽  
Limit Of Quantification ◽  
Voltammetric Sensors ◽  
Printed Sensors ◽  
Lower Background

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.

scholarly journals Determination of Lisinopril in Pure and Tablet form by Using 2-Hydroxynaphthaldehyde as Derivatizing Reagent

2021 ◽  
Vol 22 (1) ◽  
pp. 115-126
Author(s):  
Zahid Ali Zounr
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Products ◽  
Molar Absorptivity ◽  
Coefficient Of Determination ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Tablet Form ◽  
Derivatizing Reagent ◽  
Derivatization Reaction

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.

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