Investigation of the composition of anabolic tablets using near infrared spectroscopy and Raman chemical imaging

Abstract

The use of performance enhancing drugs is a widespread phenomenon in professional and leisure sports. A spectroscopic study was carried out on anabolic tablets labelled as 5 mg methandienone tablets provided by police departments. The analytical approach was based on a two-step methodology: a fast analysis of tablets using near infrared (NIR) spectroscopy to assess sample homogeneity based on their global composition, followed by Raman chemical imaging of one sample per NIR profile to obtain information on sample formulation. NIR spectroscopy assisted by a principal components analysis (PCA) enabled fast discrimination of different profiles based on the excipient formulation. Raman hyperspectral imaging and multivariate curve resolution - alternating least square (MCR-ALS) provided chemical images of the distribution of the active substance and excipients within tablets and facilitated identification of the active compounds. The combination of NIR spectroscopy and Raman chemical imaging highlighted dose-to-dose variations and succeeded in the discrimination of four different formulations out of eight similar samples of anabolic tablets. Some samples contained either methandienone or methyltestosterone whereas one sample did not contain an active substance. Other ingredients were sucrose, lactose, starch or talc. Both techniques were fast and non-destructive and therefore can be carried out as exploratory methods prior to destructive screening methods. Copyright © 2015 John Wiley & Sons, Ltd.

Recent advancement of chemical imaging in pharmaceutical quality control: From final product testing to industrial utilization

“…The PC score surface image could manifest the trend of studied indicator or sample clustering. 3,30,31 But at other times, the score surfaces do not contain any chemical meaning and the method is inadaptable, especially when coping with compositional-complex chemical images.…”

Detection of Counterfeit Durateston® Using Fourier Transform Infrared Spectroscopy and Partial Least Squares - Discriminant Analysis

“…17,20 PLS-DA is also based on the PCA decomposition, the difference being that the combinations of variables, called PLS factors or latent variables, are defined in such a way that the covariance of the instrumental data with the response variable (predefined classes) are maximized, leading to quantitative methods with low errors and high discrimination power between the different classes in discriminant analysis. 13,15,18,20 PLS-DA is performed using binary coding, in which a dummy discrete response vector y is attributed to the data set, such as 0 for counterfeit samples and 1 for original samples.…”

“…17,20 PLS-DA is also based on the PCA decomposition, the difference being that the combinations of variables, called PLS factors or latent variables, are defined in such a way that the covariance of the instrumental data with the response variable (predefined classes) are maximized, leading to quantitative methods with low errors and high discrimination power between the different classes in discriminant analysis. 13,15,18,20 PLS-DA is performed using binary coding, in which a dummy discrete response vector y is attributed to the data set, such as 0 for counterfeit samples and 1 for original samples. 14,17,21,22 In the training stage, the method is trained to assign "membership values", one for each class; a test sample is then assigned to a specific class if its y value surpasses a specific prediction threshold that may be estimated by establishing confidence limits for each sample classified.…”

“…[13][14][15]19 However, to the best of our knowledge, only one work using spectroscopic methods to analyze anabolic steroid medicines has been published so far, describing the investigation of the composition of methandrostenolone-containing tablets by near infrared and Raman spectroscopy. 20 The aim of this work was to develop a simple, fast, low-cost and reliable method for the detection of Durateston ® counterfeits using FTIR and partial least squares -discriminant analysis (PLS-DA).…”

Advancing supplement science: challenges and solutions

“…Rebiere et al . showed that the two‐step implementation of near infrared (NIR) spectroscopy and Raman chemical imaging helped detect counterfeit tablets labelled as methandienone . Further studies of counterfeit products are offered by Custers et al .…”