Quantitative Determination of Prednisone in Tablets by Infrared Attenuated Total Reflection and Raman Spectroscopy

2012 ◽  
Vol 95 (3) ◽  
pp. 744-750 ◽  
Author(s):  
Sylwester Mazurek ◽  
Roman Szostak

Abstract The quantification of prednisone in tablets was performed using partial least squares (PLS) models based on FTIR-attenuated total reflection (ATR) and FT-Raman spectra. To compare the predictive ability of these models, the relative standard error of prediction (RSEP) values were calculated. In the case of prednisone determination from the FT-Raman data, RSEP values of 3.1 and 3.2% for the calibration and validation data sets were obtained. For FTIR-ATR models, which were constructed using five spectra for each sample, these errors amounted to 2.6 and 2.9%, respectively. Four commercial products containing 1, 5, 10, and 20 mg prednisone/tablet were quantified. Concentrations derived from the elaborated models correlated strongly with the results of reference analyses and with the declared values (in parentheses). The analyses gave recoveries of 100.0–101.6% (100.1–103.0%) and 98.1–103.2% (100.4–102.9%) for FTIR-ATR and FT-Raman data, respectively. A successful quantification of prednisolone in tablets containing 5 mg active ingredient/tablet was also performed using the PLS model, which was based on FTIR-ATR spectra, with a recovery of 99.8 (98.8%). Both reported spectroscopic techniques can be used as fast and convenient alternatives to the standard pharmacopeial methods of prednisone and prednisolone quantification in solid dosage forms. However, in the case of FTIR-ATR spectroscopy, it is necessary to repeat measurements several times to obtain sufficiently low quantification errors.

2020 ◽  
Vol 45 (1) ◽  
pp. 92-103 ◽  
Author(s):  
V Bolaños-Carmona ◽  
C Benavides-Reyes ◽  
S González-López ◽  
P González-Rodríguez ◽  
P Álvarez-Lloret

SUMMARY Objectives: To compare the degree of conversion (DC) of different flowable and sculptable bulk-fill composites (BFC), at 0- and 4-mm depths from the surface, by Fourier transform infrared (FTIR), attenuated total reflection FTIR (ATR-FTIR), and FT-Raman spectroscopic techniques. Methods and Materials: Six BFC were investigated, including three sculptable composites (Admira Fusion [Voco], Aura Bulk Fill [SDI], and X-tra Fill [Voco]) and three flowable composites (Venus Bulk Fill [Heraeus], Filtek [3M], and X-tra Base [Voco]). Three molds of each composite were light cured as specified by the manufacturer. For each mold, slices corresponding to 0-mm (surface) and 4-mm depth were analyzed by spectroscopic techniques: ATR-FTIR, FTIR, and FT-Raman. The spectra of uncured composite material were used as an analytical control for background subtraction of the treated composite. The area and amplitude of the reference peaks (1607 and 1637 cm−1) were obtained to calculate the DC percentage at 0- and 4-mm depth. A Kruskal-Wallis nonparametric test was used for materials, and paired comparisons were made using Mann-Whitney nonparametric test. Wilcoxon's rank test was used for comparison between spectroscopic methods and between 0- and 4-mm depth in each composite. Significance was accepted at p<0.05. Results: FTIR showed significantly lower DC values, both in areas and amplitudes of the peaks, when compared with the results reported by different BFC. Differences between the surface and 4-mm depth were detected more precisely by FT-Raman. ATR-FTIR obtained DC values significantly higher than those obtained by FTIR. Conclusions: The vibrational spectroscopy method significantly influenced DC measurements of the flowable and sculptable BFC explored.


Processes ◽  
2020 ◽  
Vol 9 (1) ◽  
pp. 8
Author(s):  
Sylwester Mazurek ◽  
Kamil Pichlak ◽  
Roman Szostak

A quantitative analysis of vitamins A and E in commercial ointments containing 0.044% and 0.8% (w/w) of active pharmaceutical ingredients, respectively, was performed using partial least squares models based on FT Raman spectra. Separate calibration systems were prepared to determine the amount of vitamin A in a petrolatum base ointment and to quantify vitamins A and E in a eucerin base one. Compositions of the laboratory-prepared and commercial samples were controlled through a principal component analysis. Relative standard errors of prediction were calculated to compare the predictive ability of the obtained regression models. For vitamin A determination, these errors were found to be in the 3.8–5.0% and 5.7–5.9% ranges for the calibration and validation data sets, respectively. In the case of vitamin E modeling, these errors amounted to 3.7% and 4.4%. On the basis of elaborated models, vitamins A and E were successfully quantified in two commercial products with recoveries in the 99–104% range. The obtained data indicate that the Raman technique allows for accurate analysis of the composition of semisolid formulations in their native state, including low dose preparations.


2021 ◽  
pp. 000370282110643
Author(s):  
Andrea Teuber ◽  
Robert Stach ◽  
Julian Haas ◽  
Boris Mizaikoff

An innovative mid-infrared spectroscopic sensor system based on quantum cascade lasers has been developed. The system combines the versatility of substrate-integrated hollow waveguides (IHWGs) with the robustness of attenuated total reflection (ATR) crystals employed as internal reflection waveguides for evanescent field sensing. IHWGs are highly reflective metal structures that propagate infrared (IR) radiation and were used as light pipes for coupling radiation into the ATR waveguide. The combined IHWG-ATR device has been designed such that the utmost stability and robustness of the optical alignment were ensured. This novel assembly enables evanescent field absorption measurements at yet unprecedently harsh conditions, that is, high pressure and temperature. Combining these advantages, this innovative sensor assembly is perfectly suited for taking ATR spectroscopy into the field where the robustness of the assembly and optical alignment is essential.


1977 ◽  
Vol 31 (4) ◽  
pp. 289-292 ◽  
Author(s):  
Tomas Hirschfeld

In total reflection spectroscopy the effective sampled depth increases as the angle of incidence approaches the critical one. At each angle of incidence, successive layers within the sample are weighed differently in the overall spectrum, and the manner of this weighing changes with angle. It is thus possible in principle to deconvolute a set of spectra taken at different angles into spectra corresponding to successive depth invervals. As this angular effect is particularly marked near the critical angle, where attenuated total reflection spectra are severely distorted, the spectra usually require inversion into optical constant spectra. This has been done by a new technique that measures spectra twice at each angle with different prism materials to give the necessary data sets. Examples of such subsurface spectra are shown.


2013 ◽  
Vol 67 (2) ◽  
pp. 126-131 ◽  
Author(s):  
Milan Milosevic

This is an unusual paper in that it does not address a particular research topic or present a novel experimental method or a new theoretical result. This paper addresses our basic understanding of the nature of the evanescent wave, the wave that is the basis of the entire field of Attenuated Total Reflection (ATR) spectroscopy. I recently had the opportunity to reexamine the foundations of ATR spectroscopy and was surprised to have had to change my own mental picture of the evanescent wave that I have built over the last 25 years. Over the years I have had numerous discussions with a large number of workers in the field as well as with my former mentor, and one of the originators and the principal developer of ATR spectroscopy, the late N.J. Harrick. Everything brought up in all these discussions was perfectly consistent with my old mental picture of the evanescent wave. Thus, I believe that the picture of the evanescent wave that I had is virtually universally held by workers in the field. This paper describes the new picture of the evanescent wave that emerged from said reexamination process.


2011 ◽  
Vol 4 (6) ◽  
pp. 420-429 ◽  
Author(s):  
Kerstin M.-C. Hans ◽  
Susanne Müller ◽  
Markus W. Sigrist

2007 ◽  
Vol 21 (5-6) ◽  
pp. 257-268 ◽  
Author(s):  
Yiwu Zheng ◽  
Xuxin Lai ◽  
Henrik Ipsen ◽  
Jørgen Nedergaard Larsen ◽  
Henning Løwenstein ◽  
...  

It is believed that antigens should be adsorbed onto adjuvants in vaccines. The adsorption-modified structure of antigens is important to understand the mechanism of adjuvants and vaccine immunogenicity. The structural stability of antigens is of major importance. The changes in structure can be induced by degradation and/or increase of storage temperature. In this study the structural stability of two model antigens, bovine serum albumin (BSA) andβ-lactoglobulin (BLG) were compared when they were adsorbed onto aluminium hydroxide and when they were in solutions using Fourier transform infrared – attenuated total reflection (FTIR-ATR) spectroscopy. The structural stability of these two proteins was studied at different temperature and during storages. The present results showed that the structure of antigens can be stabilized by adsorption onto aluminium hydroxide. Non-adsorbed protein antigens present in vaccines may facilitate the degradation of the vaccine.


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