Forensic analysis of anabolic steroids tablets composition using attenuated total reflection Fourier transform infrared microspectroscopy (µATR‐FTIR) mapping

Abstract

The use of falsified and unregistered drugs is a worldwide public health problem.Because these global market products usually do not follow the Good Manufacturing Practices required by health legislation, its composition may be completely different from the original or may contain relevant concentrations of impurities and toxic contaminants. Since anabolic steroids are among the main irregular therapeutic classes seized in Brazil, here we propose a new methodology for analyzing these products, in tablets form, using Attenuated Total Reflection Fourier Transform Infrared Microspectroscopy (µATR-FTIR) mapping. Spectra were acquired from solid tablets by attenuated total reflection, through point mapping methodology. In data processing, a characteristic absorption band for each Active Pharmaceutical Ingredient (API) was integrated and plotted to create its distribution map. This technique was applied in an unprecedented way for the forensic analysis of anabolic steroids and proved to be effective in distinguishing falsified products based on the detection of their APIs.It was possible to detect APIs in 26 out of 30 samples, five of which were classified as falsified only through µATR-FTIR analysis. We were able to create distribution maps of the detected substances associating the microspectroscopic results with characteristic band integration method, which can be used to detect substances and to study samples' homogeneity. We concluded that this methodology is promising for the analysis of anabolic steroid tablets, and can be used in a complementary way with techniques already consolidated in forensic laboratory routine for a better classification of questioned samples between authentic and falsified ones.

Screening method for the characterization of anabolic steroids seized in Brazil using paper spray mass spectrometry and chemometric tools

“…These results are in accordance with the report that testosterone and its esters have been responsible for most of the cases of undeclared active ingredients in seized samples of anabolic steroids in Brazil. 4 The results described above were corroborated by the interpretation of PS-MS data. In all the mass spectra, except for the only one not containing anabolic steroids, the most intense ions were characteristic of the respective detected active ingredients.…”

“…There is a high prevalence of illicit trade of anabolic steroids for non‐medical use in Brazil. One of the reasons for this is that they are considered controlled substances that must be purchased only under special control medical prescription 4 . Anabolic steroids have been widely used in recent years by athletes, aiming at improving performance, and by young non‐athletes for aesthetic purposes.…”

“…One of the reasons for this is that they are considered controlled substances that must be purchased only under special control medical prescription. 4 Anabolic steroids have been widely used in recent years by athletes, aiming at improving performance, and by young non-athletes for aesthetic purposes. These drugs have also been employed to treat some diseases, such as hypogonadism and anemia.…”

“…Among these techniques, we can mention ultra-and high-performance liquid chromatography (UPLC and HPLC) with mass spectrometry or diode array UV detector, [9][10][11][12] gas chromatography coupled to mass spectrometry (GC-MS) or flame ionization detection (GC-FID), 8, [12][13][14] differential scanning calorimetry (DSC), 15 and nuclear magnetic resonance ( 1 H NMR) spectroscopy. 16 Some articles have utilized techniques based on chemical images generated by coupling a microscope with a vibrational spectroscopic technique, such as attenuated total reflection Fourier transform infrared microspectroscopy (μATR-FTIR) 4 and hyperspectral Raman spectroscopy. 17 These expensive techniques are also laborious and time consuming, requiring more complex chemometric tools and being exclusively applied to heterogenous samples, such as tablets for which distribution chemical maps can be obtained.…”

Fake anabolic androgenic steroids on the black market – a systematic review and meta-analysis on qualitative and quantitative analytical results found within the literature

“…GC–MS with [ 51 ] or without [ 40 , 46 ] prior derivatization of the AAS has also been successfully used to screen and quantify AAS, based on their fragmentation patterns and retention times. Other complementary techniques like 1H-nuclear magnetic resonance (NMR) [ 39 , 44 ], infrared (IR) spectroscopy [ 34 , 40 , 46 , 55 ], differential scanning calorimetry (DSC) [ 40 ], or high resolution/high accuracy mass spectrometry (LC-HRMS) [ 26 , 32 , 42 ] have also been used to measure AAS. For AAS, both low-resolution and high-resolution mass spectrometers were employed.…”