The Stability of 4-Chloromethcathinone in Blood and Vitreous Humor

We present results of our study on the stability of 4-chloromethcathinone (4-CMC) in authentic postmortem peripheral blood and vitreous humor samples. The stability of 4-CMC was determined in postmortem blood samples (for a period of 90 days) and vitreous humor (30 days) at three different temperatures: −15°C, +4°C, and + 23°C. The analyses were carried out using ultra-high-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS). In both materials, the lowest 4-CMC stability was demonstrated at room temperature. The blood samples stored in a freezer (−15°C) showed stability for the entire study period (90 days), while in the case of the vitreous humor sample stored at the same temperature the concentration of the substance decreased by 53% after 30 days. The study carried out in authentic postmortem blood and vitreous humor samples confirms the previous reports of 4-CMC instability in biological material. Authors suggest that the biological material should be stored frozen until analyses are carried out as soon as possible after collection of the material.     

Empirical Evaluation of the Reliability of Photogrammetry Software in the Recovery of Three-Dimensional Footwear Impressions

This paper examines the reliability of Structure from Motion (SfM) photogrammetry as a tool in the capture of forensic footwear marks. This is applicable to photogrammetry freeware DigTrace but is equally relevant to other SfM solutions. SfM simply requires a digital camera, a scale bar, and a selection of oblique photographs of the trace in question taken at the scene. The output is a digital three-dimensional point cloud of the surface and any plastic trace thereon. The first section of this paper examines the reliability of photogrammetry to capture the same data when repeatedly used on one impression, while the second part assesses the impact of varying cameras. Using cloud to cloud comparisons that measure the distance between two-point clouds, we assess the variability between models. The results highlight how little variability is evident and therefore speak to the accuracy and consistency of such techniques in the capture of three-dimensional traces. Using this method, 3D footwear impressions can, in many substrates, be collected with a repeatability of 97% with any variation between models less than ~0.5 mm.     

Detection of Mitragynine in Mitragyna Speciosa (Kratom) Using Surface-Enhanced Raman Spectroscopy with Handheld Devices

A simple, quick, selective, sensitive, and effective field-friendly method capable of being used by nonexperts has been developed for detecting mitragynine in Mitragyna speciosa (kratom) using surface-enhanced Raman spectroscopy (SERS). Over 100 samples and blanks (known to be either positive or negative for the presence of mitragynine) were examined in duplicate using five identical handheld Raman spectrometers, which provided a data set of over 1,000 examinations. Based on the results of these analyses, the method yielded a true-positive rate of 99.3%, a true-negative rate of 97.9%, a false-positive rate of 2.1%, and a false-negative rate of 0.7%. The average minimum detectable concentration (C_m) of mitragynine that reproducibly yielded a match for one of the library spectra on all five instruments was determined to be 342 ng/mL (ppb). This C_m value is a conservative estimate considering that the extraction process was not fully optimized by this study, which was not necessary since the C_m value achieved was well below typical mitragynine concentrations in kratom (1.3–2.3%). The method is ideal (i) for prioritizing samples for additional testing using other more time-consuming laboratory-based techniques needed to detect and quantify mitragynine and (ii) for field use at international mail facility (IMF) satellite laboratories to help interdict kratom and prevent this dangerous product from reaching the U.S. supply chain.     

Postmortem Changes of Female External Genitalia and Their Importance in Suspected Sexual Abuse

Examination of the female external genitalia to assess for sexual abuse is performed in living individuals, and the interpretation of the findings is based on evidence-based studies. However, in the deceased, no such studies are available, and postmortem changes could present as suspicious findings that can be mistaken for trauma. Patches of discoloration in the hymen were reported previously in one case as hypostasis (i.e., livor and lividity), and based on this finding, it was listed as a finding that is not associated with trauma. This was a retrospective study that was conducted in the Center of Forensic and Legal Medicine in Dammam, Saudi Arabia over a 4-year period. The study included 30 deceased women in whom photographic documentation of their external genitalia was assessed for postmortem changes. The postmortem interval ranged from less than 24 h to more than 100 days, and the ages of these deceased women were in the 20–40 year-old age group. In cases where the hymen, vagina, and/or fossa navicularis were clearly visible, none of these areas showed any hypostatic discoloration. A comparison between antemortem and postmortem appearance of the hymen in one case clearly showed the absence of hypostatic changes in the hymen. In conclusion, any discoloration of the external genitalia that is detected in a female decedent requires serious consideration.     

Postmortem Computed Tomography and Magnetic Resonance Imaging of Gunshot Wounds to the Neck

Postmortem magnetic resonance imaging (MRI) is rarely used for the radiologic assessment of gunshot injuries, although it has clear advantages over postmortem computed tomography (CT) with regard to the imaging of soft tissue injuries. Another benefit in using MRI is that lodged projectiles composed of nonferromagnetic material such as lead present only marginal metal artifacts compared with severe artifacts on CT. This case report presents CT and MRI findings in a case with two gunshot wounds to the neck: a perforating wound and a nonperforating wound with a lead bullet lodged in the cervical spine. The decedent underwent CT and MRI before the scheduled autopsy. A ring of radiopaque material under the dermis in the fatty tissue was identified at both entrance wounds on CT, which was indicative of contact shots. The perforating gunshot was clearly indicated on CT by bullet fragments along the wound channel through the perforated 6th cervical vertebra and the fractured cricoid cartilage at the exit wound. The second trajectory, however, was only assumed based on the presence of gunshot residues at the entrance wound and the position of the lodged bullet. The radiologic assessment was severely impeded by the metal artifacts on CT. Barely noticeable metal artifacts on MRI allowed for clear visualization of the soft tissue injuries and the ruptured medulla oblongata. Only MRI clarified the soft tissue injuries of the brainstem noninvasively, which could provide specific and graphic information on the rapidity of death and the incapacitation of the victim.     

Volatile Organic Compounds,Spectral Characterization and Morphology of Ammonium Nitrate Fuel Oil (ANFO) Samples

Ammonium nitrate fuel oil is an explosive mixture found in most antipersonnel landmines (APL) buried throughout the Colombian territory. During more than 50 years of internal conflict, the Colombian government has found that trained dogs are the most effective method to detect APL. However, the olfactive signature in ANFO is unknown and also if there are differences in detection related to the explosive manufacturing origin. Therefore, this work begins with the analytical validation of the method used to determine ammonia, in its derivatized form as carbamate, released by home-made ANFO using HS-SPME-GC-FID. Once validated, the method was used to identify ammonia and other organic volatile compounds present in ANFO, under laboratory and simulated field conditions. The validation process includes the evaluation of the optimum conditions for the derivation and extraction of butylcarbamate, the determination of the working ranges with linear response in FID, the limits of detection and quantification, the sensitivity, and the precision. The results of the validation established linearity and sensitivity in a concentration between 20 and 120 mg/L, as well as low limits of detection and quantification of 6.4 and 21.4 mg/L, respectively. Also, an intermediate precision of 11% for butylcarbamate with a repeatability of 8%. The validated method showed in real samples of home-made ANFO besides ammonia, the presence of low molecular methylamines, and also exhibited differences in volatile compositions according to the origin. The objective of this work is to offer a reliable analytical methodology for the extraction and analysis of volatile compounds from ANFO.     

Combined Collection and Analysis of Inorganic and Organic Gunshot Residues

Gunshot residue (GSR) analysis and their interpretation provide crucial information on a criminal investigation involving the use of firearms. To date, several approaches have been proposed for the implementation of a combined sampling and analysis of inorganic (IGSR) and organic GSR (OGSR). However, it is not clear at this stage if concurrent analyses of both types of residue might be detrimental to the analysis of IGSR currently applied in forensic laboratories. Thus, this work aims to compare and evaluate three different protocols for the combined collection and analysis of IGSR and OGSR. These methods, respectively, involve the use of a modified stub (with two halves, one for the detection of IGSR and the other for the analysis of OGSR); the sequential recovery of GSR with two stubs mounted with different adhesives (double-sided carbon tape and Tesa® TACK) and the sequential analysis of IGSR and OGSR from a single carbon stub following carbon deposition. The detection of IGSR was carried out using SEM-EDX, while OGSR analysis was performed using ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Obtained results for experiments performed using Geco Sinoxid^® ammunition indicated that sequential analysis was the most suitable protocol for the combined collection and analysis of both IGSR and OGSR. A higher number of inorganic (characteristic and consistent) particles and higher concentrations of ethylcentralite, N-nitrosodiphenylamine, diphenylamine, and nitroglycerin were recovered with this method.     

Determining Line-Crossing Sequences Between Laser Printing and Writing Pen Using Coaxial Light

Determining the application sequence of hand-written pen ink and printer toner lines has attracted significant interest in questioned document examination. This study uses coaxial light to determine line-crossing sequences, with intersections observed under a VSC600 forensic document workstation and a Leica M205A Stereo-microscope. Results show that reflected light at intersections and color contrast between intersections and nonintersections was observed when a hand-written ink line passes over a toner line, while a toner line passing over a written line appeared dull, with no color contrast. The procedure was tested under a range of conditions, such as types of writing pens and laser printers, the writer, and writing pressure, with the latter playing an important role in the evaluation. To validate the results, a 90% detection rate and 98% accuracy rate were achieved from 50 samples of blind testing, which is more effective than optical microscopy.     

Nondestructive Differentiation of Polyester Single White Fibers Using Synchrotron Radiation Microbeam X-ray Fluorescence Spectrometry with Vertical Focusing

In this study, the nondestructive differentiation of individual white polyester clothing fibers was accomplished via synchrotron radiation microbeam X-ray fluorescence (SR-μ-XRF) analysis. SR-μ-XRF with vertical focusing is a useful nondestructive method for the analysis of a single polyester clothing fiber. Kirkpatrick–Baez (KB) mirror was used to vertically focus 20 keV X-rays for the analysis of 22 individual white polyester fibers taken from clothing commonly sold in Japan. SR-μ-XRF with a vertical focused 2 μm (V) × 300 μm (H) beam was approximately 12.8 times more sensitive than SR-XRF with an unfocused 300 μm (V) × 300 μm (H) beam for the detection of elements in single fibers. The minimum detection limits (MDLs) of the SR-μ-XRF method were 8.15 ppm for Cl and 0.06 ppm for Br. In addition to Ti in TiO₂ delustering agents, Zr and Nb impurities in the delustering agents were detected in individual fibers. Sb from a polymerization catalyst and Co from a transesterification catalyst were also detected in individual fibers. Comparing the Ti K_β/Sb L_α,β and Zr K_α/Nb K_α X-ray intensity ratios was a useful way to distinguish individual clothing fibers, and 98% of the fibers were differentiated when additional trace elements were used as discrimination indicators.     

Chemical Imaging of Human Fingermark by X-ray Photoelectron Spectroscopy (XPS)

X-ray photoelectron spectroscopy (XPS) is a widely used technique to characterize the surface chemistry of materials. It plays a crucial role in accessing qualitative and quantitative information and in detecting the presence of chemical functional groups on the surface of any material. The forensic methods available to detect and identify elements and organic/inorganic compounds are often destructive, so evidence cannot be re-analyzed. However, XPS allows rapid analysis of samples without damaging them. Recently, an increasing number of forensic researchers have begun to study certain chemical information on fingermarks. In this study, the authors aimed to present the applicability and power of XPS imaging in fingermark analysis which can also provide specific information about the fingermark chemical composition. Herein, monochromated X-ray (Al Kα) spot size was fixed at 50 μm. XPS mapping resulted in the acquisition of spectra at each pixel, in an array of 41 × 30 pixels with a step size of 50 μm. Then, a simple discussion has been made about how the scanned surface spectrum and basic snapshot spectra are used to identify different components at a fingertip of a scanned surface area (~3 mm²). Hence, a fingermark pattern contaminated with caffeine, TiO₂, and Pb/PbO deposited on the silicon wafer can be chemically mapped and visualized by XPS using principal component analysis (PCA). Thus, the present study showed the possible applicability of XPS for the identification of illicit drugs of abuse, gunshot residue, and skin care products on latent fingermark by mimicking a crime scene evidence.