Reverse engineering of formaldehyde in cosmetic products using rp-hplc technique by derivatization with 2, 4-dinitrophenylhydrazine

Author(s):  
R. AMBADEKAR SUSHAMA ◽  
BABURAO NIKAM DEEPAK ◽  
B. WARKAR CHANDAN
2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.


Author(s):  
Noreldin S. Y. Abdolla ◽  
Suad K. Omar ◽  
Ibrahim H. Habib ◽  
Hana S. Mohamed

A fast and sensitive chromatographic RP–HPLC technique for examining tramadol hydrochloride (TRM-HCl) in tablets through using fluorescence detection (FL-D) and ultraviolet detection (UV-D) is reported in this paper. The separation was carried out using the reverse phase method on a Brownlee BIO C18 analytical column with a mobile phase consisting of 0.1% acetic acid and acetonitrile (2.5:7.5 v/v), which was pumped with an isocratic elution at a flow rate of 1 ml/min. The LOD and LQD values obtained in the current study indicate that FL-D is more sensitive, and hence preferable to UV detectors in the quantification of TRM-HCl tablets over the entire concentration range used (5-125 µg/ml). The study showed that the mean percentage recoveries from five samples were 99.93-100.023% (FL-D), which is somewhat similar to that of the UV-D (99.93-100.028). In conclusion, although Fl-D is acceptable for the quantification of tramadol tablets, UV-D offers higher detection sensitivity and reproducibility, particularly within concentrations that are low in the deposit collectors.


2020 ◽  
Vol 11 (SPL4) ◽  
pp. 292-295
Author(s):  
Smitha M ◽  
Kal Satyavathi Devi ◽  
Virendra Kumar ◽  
Jaffar Hussain

A new sensitive, specific, direct, exact and correct RP-HPLC technique is established and authenticated to estimate Levetiracetam in Majority and Pharmaceutical Tablet Formulations. An isocratic, turned around period HPLC system might have been created should differentiate the pill starting with the corruption products, Phenomenex Gemini 5µ C18 (2) 100A (250 x 4.60mm, 5 µ) section. Hamilton syringe (705 NR, 50 µL) might have been utilized to injecting example Furthermore standard result. The versatile stage comprises about mixture of Methanol: Acetonitrile in the proportion (90:10 v/v) toward A stream rate about 1.0 ml /min. UV identification might have been performed toward 210 nm. The linearity might have been made for Levetiracetam in the extent from claiming 5- 30µg/ml for relationship coefficient about 0.9997. LOD Also LOQ were found will make 0.076µg/ml Furthermore 0.23µg/ml individually. Maintenance duration of the time of Levetiracetam were found with make 2.281min and 2.274min. % recuperation might have been discovered on be 99.78-100.45 What's more %RSD might have been found for over ±2. Those system needs been approved as stated by ICH rules to linearity, precision, accuracy, robustness, ruggedness, LOD furthermore LOQ. Those produced approved system might have been effectively connected to dependable quantification about Levetiracetam to mass and pharmaceutical measurement type.


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