scholarly journals DSC, FT-IR, NIR, NIR-PCA and NIR-ANOVA for determination of chemical stability of diuretic drugs: impact of excipients

2018 ◽  
Vol 16 (1) ◽  
pp. 116-132 ◽  
Author(s):  
Anna Gumieniczek ◽  
Hanna Trębacz ◽  
Łukasz Komsta ◽  
Agnieszka Atras ◽  
Beata Jopa ◽  
...  
Keyword(s):  
High Temperature ◽  
Citric Acid ◽  
Principal Component ◽  
Magnesium Stearate ◽  
Scanning Calorimetry ◽  
Diuretic Drugs ◽  
Temperature And Humidity ◽  
Ft Ir ◽  
Selection Of

AbstractIt is well known that drugs can directly react with excipients. In addition, excipients can be a source of impurities that either directly react with drugs or catalyze their degradation. Thus, binary mixtures of three diuretics, torasemide, furosemide and amiloride with different excipients,i.e. citric acid anhydrous, povidone K25 (PVP), magnesium stearate (Mg stearate), lactose, D-mannitol, glycine, calcium hydrogen phosphate anhydrous (CaHPO4) and starch, were examined to detect interactions. High temperature and humidity or UV/VIS irradiation were applied as stressing conditions. Differential scanning calorimetry (DSC), FT-IR and NIR were used to adequately collect information. In addition, chemometric assessments of NIR signals with principal component analysis (PCA) and ANOVA were applied.Between the excipients examined, lactose and starch did not show any interactions while citric acid, PVP, Mg stearate and glycine were peculiarly operative. Some of these interactions were shown without any stress, while others were caused or accelerated by high temperature and humidity, and less by UV/VIS light. Based on these results, potential mechanisms for the observed interactions were proposed Finally, we conclude that selection of appropriate excipients for torasemide, furosemide and amiloride is an important question to minimize their degradation processes, especially when new types of formulations are being manufactured.

scholarly journals Determination of Chemical Stability of Two Oral Antidiabetics, Metformin and Repaglinide in the Solid State and Solutions Using LC-UV, LC-MS, and FT-IR Methods

Molecules ◽  
2019 ◽  
Vol 24 (24) ◽  
pp. 4430
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka-Rycerz ◽  
Tomasz Mroczek ◽  
Krzysztof Wojtanowski
Keyword(s):  
High Temperature ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Magnesium Stearate ◽  
Oral Antidiabetics ◽  
First Order ◽  
First Order Kinetics ◽  
Ft Ir ◽  
The Stability

Firstly, metformin and repaglinide were degraded under high temperature/humidity, UV/VIS light, in different pH and oxidative conditions. Secondly, a new validated LC-UV method was examined, as to whether it validly determined these drugs in the presence of their degradation products and whether it is suitable for estimating degradation kinetics. Finally, the respective LC-MS method was used to identify the degradation products. In addition, using FT-IR method, the stability of metformin and repaglinide was scrutinized in the presence of polyvinylpyrrolidone (PVP), mannitol, magnesium stearate, and lactose. Significant degradation of metformin, following the first order kinetics, was observed in alkaline medium. In the case of repaglinide, the most significant and quickest degradation, following the first order kinetics, was observed in acidic and oxidative media (0.1 M HCl and 3% H2O2). Two new degradation products of metformin and nine new degradation products of repaglinide were detected and identified when the stressed samples were examined by our LC-MS method. What is more, the presence of PVP, mannitol, and magnesium stearate proved to affect the stability of metformin, while repaglinide stability was affected in the presence of PVP and magnesium stearate.

scholarly journals Compatibility Studies of Valsartan with Different Pharmaceutical Excipients

2019 ◽  
Vol 70 (7) ◽  
pp. 2590-2600
Author(s):  
Ioana Cristina Tita ◽  
Lavinia Lupa ◽  
Bogdan Tita ◽  
Roxana Liana Stan ◽  
Laura Vicas
Keyword(s):  
Magnesium Stearate ◽  
Dosage Forms ◽  
Compatibility Studies ◽  
Scanning Calorimetry ◽  
Pharmaceutical Dosage Forms ◽  
Lactose Monohydrate ◽  
Pharmaceutical Excipients ◽  
Solid Dosage ◽  
Fourier Transformed Infrared Spectroscopy ◽  
Ft Ir

Compatibility studies between active drugs and excipients are substantial in the pharmaceutical technology. Thermal analysis has been extensively used to obtain information about drug-excipient interactions and to perform pre-formulation studies of pharmaceutical dosage forms. The objective of the present study was to evaluate the compatibility of the valsartan (VALS) with pharmaceutical excipients of common use including diluents, binders, disintegrants, lubricants and solubilising agents. Thermogravimetry (TG), derivative thermogravimetry (DTG), but especially differential scanning calorimetry (DSC) were used for a first screening to find small variations in peak temperature and/or their associated enthalpy for six drug/excipient mixtures (starch, cross caramelose sodique, microcrystalline cellulose 102, povidone K30, lactose monohydrate and magnesium stearate), which indicate some degree of interaction. Additional methods using Fourier transformed infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRPD) confirmed the incompatibility of VALS with starch, povidone K30, lactose monohydrate and magnesium stearate. Those excipients should be avoided in the development of solid dosage forms.

Compatibility between Magnesium Stearate and Pharmaceutical Acidic Active Compounds/Excipients with DSC

2020 ◽  
Vol 856 ◽  
pp. 190-197
Author(s):  
Pornsit Chaiya ◽  
Thawatchai Phaechamud
Keyword(s):  
Differential Scanning Calorimetry ◽  
Magnesium Stearate ◽  
X Ray Diffraction ◽  
Salt Form ◽  
Scanning Calorimetry ◽  
Powder Mixtures ◽  
X Ray ◽  
Pharmaceutical Excipients ◽  
Drug Compounds ◽  
Ft Ir

Compatibility investigation was performed between magnesium stearate and acidic drug compounds (ibuprofen, indomethacin and valproic acid) and acidic pharmaceutical excipients (lactic acid and citric acid) using differential scanning calorimetry (DSC). DSC study indicated the possible incompatibility for the mixture between magnesium stearate and any compounds. Alteration in DSC thermogram was found in all mixtures. The eutectic phenomenon was found in the powder mixture of magnesium stearate and ibuprofen. In addition, the presence of melting endothermic peak of stearic acid in other powder mixtures except the mixture of magnesium stearate and indomethacin indicating breakage of salt form of magnesium stearate. This alteration could relate to the influence on physicochemical properties of drug compounds and pharmaceutical excipients which powder x-ray diffraction (PXRD) and Fourier Transform Infrared Spectroscopy (FT-IR) should be further analyzed to confirm the interactions between compounds.

Chemometric Approach to a Rapid Attenuated Total Reflection Fourier Transform Infrared Analysis of Complex Heroin-Based Mixtures

2020 ◽  
pp. 000370282096971
Author(s):  
Nataša Radosavljević Stevanović ◽  
Milena Jovanović ◽  
Federico Marini ◽  
Slavica Ražić
Keyword(s):  
Principal Component Analysis ◽  
Fourier Transform ◽  
Principal Component ◽  
Fourier Transform Infrared ◽  
Total Reflection ◽  
Attenuated Total Reflection ◽  
Illegal Market ◽  
Ft Ir

Heroin is one of the most frequently seized drugs in Southeastern Europe. Due to the position in the Balkan route, the Republic of Serbia keeps important role in suppression of the trafficking of heroin for domestic and foreign illegal market. This research is aimed to provide a good scientific approach in the field of seized heroin analysis. Two different forms of heroin are present in the illegal market, mostly in mixtures with typical “cutting” agents: caffeine, paracetamol, and sugars. It was observed that the quantity of pure heroin in seized samples slightly increases from year to year. The aim of this study was to produce a reliable and fast procedure for classification of illicit heroin samples and determination of the concentration range of heroin in the samples. For that purpose, the attenuated total reflection Fourier transform infrared spectroscopy (ATR FT-IR) technique was used and combined with such chemometric methods as principal component analysis, cluster analysis, and partial least squares. Principal component analysis (PCA) as an unsupervised model was used for exploratory purposes to identify trends, similarities, and differences between samples by reducing the dimensionality of the data. The cluster classification of examined samples turned out to be extremely useful to evaluate the possibilities of the ATR FT-IR technique to classify the samples appropriately into the patterns, the constituted clusters. Additionally, partial least square was the suitable method for the purpose of determination of the heroin hydrochloride concentration range in examined samples. It is proved that the joined application of spectroscopy and chemometrics can be extremely convenient and useful for forensic and drugs control laboratories.

scholarly journals Determination of polydextrose as a fat replacer in butter

2008 ◽  
Vol 25 (No. 1) ◽  
pp. 25-31 ◽  
Author(s):  
K. Míčková ◽  
J. Čopíková ◽  
A. Synytsya
Keyword(s):  
Citric Acid ◽  
Ir Spectroscopy ◽  
Petroleum Ether ◽  
Solid Fraction ◽  
Condensation Product ◽  
Large Excess ◽  
Fat Replacer ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Polydextrose is used in several countries as a low caloric sugar and fat substitute (bulking agent). It is prepared by condensation of glucose, D-glucitol, and citric acid (89:10:1). The resulting condensation product has no chemically defined structure but it represents a mixture of polymerisation products. The determination of polydextrose in butter is complicated owing to a large excess of fats and to the presence of other compounds, mainly proteins. FT-IR spectroscopy seems to be a satisfying method for the detection of polydextrose in samples derived from food products. The presence of polydextrose in butter was verified after the removal of fats by extraction with petroleum ether and deproteinisation with Sevag reagent, CHCl3/<i>n</i>-butanol (v/v = 4:1) mixture, or trichlorocetic acid. The solid fraction of butter and butter containing a known amount of polydextrose were prepared and analysed by FT-IR spectroscopy. IR marker bands of polydextrose centred at 1150, 1076 and 1040 cm<sup>&minus;1</sup> were found only in the case of the sample of butter with polydextrose.

scholarly journals Synthesis of a new organic probe 4-(4 acetamidophenylazo) pyrogallol for spectrophotometric determination of Bi(III) and Al(III) in pharmaceutical samples

2021 ◽  
Vol 40 (1) ◽  
pp. 108-126
Author(s):  
Jumana W. Ammar ◽  
Zainab A. Khan ◽  
Marwa N. Ghazi ◽  
Naser A. Naser
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Scanning Calorimetry ◽  
Spectrophotometric Methods ◽  
Modern Development ◽  
Relative Standard ◽  
Visible Spectra ◽  
Ft Ir ◽  
Linear Solvation Energy

Abstract A modern development discusses the synthesis and validity of simple, sensitive, and versatile spectrophotometric methods for Bi(III) and Al(III) determination in pharmaceutical formulations have been conducted. In the present paper, 4-(4 acetamidophenylazo) pyrogallol has been synthesized as a new organic compound, 4-APAP, by coupling pyrogallol in a regulated pH medium with diazotized p-aminoacetanilide. 4-APAP was identified by methods of FT-IR, 1H-NMR, 13C-NMR, and thermal analysis (thermogravimetry and differential scanning calorimetry). Solvatochromic activity was also studied in solvents with different polarities. The Kamlet and Taft linear solvation energy relationship was used to correlate shifts in UV-Visible spectra of 4-APAP with Kamlet-Taft parameters (α, β, and π*). The optimum assay conditions showed linearity from 0.3–13 to 0.5–11 μg·mL−1 for Bi(III) and Al(III), respectively. Molar absorptivity values were 3.365 × 104 and 0.356 × 104 L·mol−1·cm−1 for Bi(III) and Al(III), with similar Sandell's sensitivity measures of 0.006 and 0.008 μg·cm−2. Detection limits and quantification limits were 0.013 and 0.043 μg·mL−1 for Bi(III), respectively, and 0.018 and 0.059 μg·mL−1 for Al(III) with the relative standard deviation for determination of both metal ions using 4-APAP probe being <2.0%. The validity, accuracy, and efficiency of the approaches were demonstrated by the determination of Bi(III) and Al(III) in different formulations.

scholarly journals THE INFLUENCE OF REACTION TIME ON THE PROPERTIES OF MICROWAVE SYNTHESIZED POLY(LACTIDE)

2019 ◽  
Vol 10 (1) ◽  
Author(s):  
Ivan Ristić ◽  
Milovan Jotanović ◽  
Tamara Erceg ◽  
Ljubiša Nikolić ◽  
Suzana Cakić ◽  
...  
Keyword(s):  
Reaction Time ◽  
Renewable Resources ◽  
Gel Permeation Chromatography ◽  
Polymer Materials ◽  
Scanning Calorimetry ◽  
Complete Life Cycle ◽  
Ft Ir ◽  
Synthesis Routes ◽  
Plant Feedstock

The consequence of drastic reduction in fossil fuel reserves has forced the scientific community to find and develop new ways to exploit renewable resources and optimize the process of polymer materials production. The aim is to obtain applicable polymer whose complete life cycle is set in ecological framework. Poly(lactide) (PLA) meets these requirements as biodegradable polyester whose monomer is derived from the plant feedstock containing carbohydrates. PLA could be prepared using the different synthesis routes, but from the point of energy saving, as well as environmental protection, the microwave synthesis of PLA is the best solution. In this work, poly(L-lactide) were synthesized in microwave reactor. Reaction time was varied, while the other parameters of the synthesis were constant. The structures of obtained polymers were confirmed by Fourier – transform infrared spectroscopy (FT-IR). For determination of molar masses of poly(L-lactide) samples, the gel permeation chromatography (GPC) was applied. Thermal properties were investigated by differential scanning calorimetry (DSC).

scholarly journals Determination of Phase Transition by Principal Component Analysis Applied to Raman Spectra of Polycristalline BATIO3 at Low and High Temperature

2012 ◽  
Vol 10 (1) ◽  
Author(s):  
E.V. Mejía-Uriarte ◽  
R.Y. Sato-Berrú ◽  
M. Navarrete ◽  
O. Kolokoltsev ◽  
J. M. Saniger
Keyword(s):  
Phase Transition ◽  
Principal Component Analysis ◽  
High Temperature ◽  
Raman Spectra ◽  
Principal Component ◽  
Component Analysis ◽  
Para Determinar

Este trabajo describe el análisis de las componentes principales (PCA) aplicados a los espectros Raman del BaTiO3como función de la temperatura. Durante el experimento las muestras fueron calentadas continuamente y losespectros Raman fueron registrados cada 0.5 °C a una razón de 0.1 °C por minuto. Este procedimiento es aplicadopara muestras de polvo compacto de BaTiO3 para obtener su comportamiento térmico de -190 °C a 230 °C. Latécnica del PCA fue capaz de distinguir características espectrales para determinar la temperatura de la transición defase y la historia térmica completa, incluyendo las transiciones de fase estructural: romboédrica a ortorrómbica at -100 °C, ortorrómbica a tetragonal at -5°C y tetragonal a cúbica at 121 °C.

scholarly journals Synthesis of Poly (Citric Acid-Co-Glycerol) and Its Application as an Inhibitor of CaCO3 Deposition

Materials ◽  
2019 ◽  
Vol 12 (22) ◽  
pp. 3800
Author(s):  
Hala Zahlan ◽  
Waseem Sharaf Saeed ◽  
Radwan Alrasheed ◽  
Naser M. Alandes ◽  
Taieb Aouak
Keyword(s):  
Citric Acid ◽  
Calcium Carbonate ◽  
Inhibition Efficiency ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Hyperbranched Polyesters ◽  
Scale Inhibition ◽  
Analysis Measurement ◽  
Ft Ir ◽  
Thermal Polycondensation

This investigation determined a feasible route to prepare hyperbranched polyesters involving citric acid (CA) and glycerol (GLC) monomers (CA-co-GLC) using a thermal polycondensation method. The synthesized copolymer was characterized using Fourier transform infrared spectroscopy (FT-IR), carbon-13 nuclear magnetic resonance spectroscopy, and differential scanning calorimetry. The ability of CA-co-GLC to inhibit deposition of inorganic scales such as calcium carbonate was investigated under varying temperature and pH medium. The evaluation of inhibition efficiency (IE) was conducted using the static scale inhibition method. The mechanism of the inhibitor’s action was investigated via growth solution analysis, measurement conductivity, and analysis of CaCO3 using FT-IR and scanning electron microscopy. The results obtained showed that the CA-co-GLC had good IE at an elevated temperature reaching 75% at 100 °C, pH 7.5, and 10 ppm copolymer dose. Using the same dose, the IE reached 66% at 50 °C and pH 10. The CA-co-GLC did not chelate Ca2+ in water, but led to a change in polymorphism, making it brittle and able to slip easily from the surface. Its action principally prevented the adhesion of calcium carbonate onto the surface.

Determination of the Percentage of Homopolymer Component in Ziegler/Natta Catalyst Linear Low-Density Polyethylene Resins Using High-Temperature Cell Fourier Transform Infrared and Partial Least Squares Quantitative Analysis Technique

2005 ◽  
Vol 59 (3) ◽  
pp. 300-304 ◽  
Author(s):  
Marlee Cossar ◽  
Joo Teh ◽  
Annikki Kivisto ◽  
Jason Mackenzie
Keyword(s):  
Fourier Transform ◽  
High Temperature ◽  
Quantitative Analysis ◽  
Ir Spectrum ◽  
Low Density Polyethylene ◽  
Low Density ◽  
Linear Low Density Polyethylene ◽  
Analysis Technique ◽  
Ft Ir

A new method for the determination of the percentage of homopolymer component, using high-temperature cell Fourier transform infrared (FT-IR) by partial least squares (PLS) quantitative analysis technique, was developed and applied to Ziegler Natta linear low-density polyethylene (LLDPE). The method is based on the IR spectrum changes between the 730 cm−1 band and 720 cm−1 band at the temperature of 110 °C, which is near the melting point of the polyethylene. The HD% (the percentage of high-density component, i.e., the percentage of homopolymer component) results obtained by CTREF (CRYSTAF in TREF mode) technique are used as the input data together with the respective FT-IR spectra for PLS analyses to establish a calibration curve. The PLS quality is characterized by a correlation coefficient of 0.997 (cross-validation) using four factors and a root mean square error of calibration (RMSEC) of 0.772. The HD% of the unknown can then be predicted by the PLS software from the unknown FT-IR spectrum. A control resin was tested seven times by CTREF and FT-IR. The HD% of the control resin was 28.59 ± 0.88% by CTREF and 29.05 ± 2.37% by FT-IR. It was found that the method was applicable for the same comonomer type of LLDPE within a melt index range and density.

Sign in / Sign up

Export Citation Format

Share Document