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Purpose Since the 1980s, the detection sensitivity of mass spectrometers has increased by improving the analysis of drugs in hair. Accordingly, the number of hair strands required for the analysis has decreased. The length of the hair segment used in the analysis has also shortened. In 2016, micro-segmental hair analysis (MSA), which cuts a single hair strand at a 0.4-mm interval corresponding to a hair growth length of approximately one day, was developed. The advantage of MSA is that the analytical results provide powerful evidence of drug use in the investigation of drug-related crimes and detailed information about the mechanism of drug uptake into hair. This review article focuses on the MSA technique and its applications in forensic toxicology. Methods Multiple databases, such as SciFinder, PubMed, and Google, were utilized to collect relevant reports referring to MSA and drug analysis in hair. The experiences of our research group on the MSA were also included in this review. Results The analytical results provide a detailed drug distribution profile in a hair strand, which is useful for examining the mechanism of drug uptake into hair in detail. Additionally, the analytical method has been used for various scenarios in forensic toxicology, such as the estimation of days of drug consumption and death. Conclusions The detailed procedures are summarized so that beginners can use the analytical method in their laboratories. Moreover, some application examples are presented, and the limitations of the current analytical method and future perspectives are described.

Purpose We previously developed evaluation methods using micro-segmental analysis (MSA) to examine the effects of external environments on drug content in hair and nails. In this study, the effects of the natural environmental factors (water, temperature, humidity, light, and soil) on drug contents in nails were examined and compared with our previous experimental data on hair. Methods Four hay-fever medicines were used as model drugs (fexofenadine, epinastine, cetirizine, and desloratadine) to evaluate drug stability in the nails. Reference nails containing the four medicines were collected from patients with hay fever who ingested the medicines daily for four months. The nails were exposed to various natural environments for up to four months. Results The effects of temperature, humidity, and light on drug contents in the nails were comparatively small. Soil significantly decomposed the nail surfaces and decreased the drug content of the nails (up to 17 %). Water also decreased the drug content (up to 12 %), although no apparent changes in nail surfaces were observed. Conclusions In comparison with hair data obtained under the same environmental conditions, light affected drugs in the hair rather than in nails, whereas water and soil greatly affected drugs in the nails rather than in hair. Although the disposition of drugs incorporated in the tissues differed between nails and hair, the analytes were detected in nails and hair strands left in severe natural environments. MSA could be useful for estimating drug-use histories and personal profiles using the nails and hair of a corpse.

Purpose Since the mid-2010s, lysergic acid diethylamide (LSD) analogs made for substance abuse have periodically emerged. In this case, three pieces of blotter paper labeled “1D-LSD” and presumably impregnated with this LSD analog, were seized. Several websites indicate that 1D-LSD is 1-(1,2-dimethylcyclobutane-1-carbonyl)-LSD. Because this analog is much more difficult to synthesize than previously reported LSD analogs, we doubted that the blotter paper contained 1D-LSD. Herein, we determined the structure of the absorbed compound. Methods One of the seized specimens was extracted and analyzed using gas chromatography/mass spectrometry (GC/MS), liquid chromatography/mass spectrometry (LC/MS), high-resolution mass spectrometry (HRMS), and nuclear magnetic resonance (NMR) spectroscopy to estimate the extract components. The estimated compound was then synthesized, yielding an authentic standard. The contents of the seized specimens were identified using authentic standard analysis with GC/MS, LC/MS, and NMR spectroscopy. Results Instrumental analyses confirmed the active compound to be 1-(thiophene-2-carbonyl)-LSD, which was inconsistent with the labeling on drug-infused blotter paper. Conclusion As in this case, similar blotter paper analyses should consider the possibility of a mismatch between the label and ingredient. To the authors’ knowledge, this is the first case report in which 1-(thiophene-2-carbonyl)-LSD was seized and the first seizure of an LSD analog in which an aromatic carboxylic acid had been condensed to LSD. This type of lysergamide may become prevalent in the near future, and we should remain alert for newly appearing lysergamides.

Purpose Micro-segmental hair analysis (MSA), which enables detailed measurement of the distribution of drugs in a single hair strand, is useful for examining the day of death and drug use history of a person. However, corpses are often found in severe environments, such as soil and freezers, which affect the drug contents in hair. Therefore, we examined the effects of temperature, humidity, light, and soil on drug stability in hair as a preliminary study to estimate personal profiles using MSA of corpse hair. Methods Four hay-fever medicines (fexofenadine, epinastine, cetirizine, and desloratadine) were used as model drugs to evaluate drug stability in hair. Reference hair strands consistently containing the four medicines along the hair shaft were collected from patients with hay-fever who ingested the medicines daily for 4 months. The hair strands were placed in chambers with controlled temperatures (− 30 to 60 °C) and relative humidities (ca. 18 % and > 90 %), exposed to light (sunlight and artificial lights) or buried in soil (natural soil and compost). Results Sunlight and soil greatly decomposed the hair surfaces and decreased the drug contents in hair (up to 37 %). However, all analytes were successfully detected along the hair shaft, reflecting the intake history, even when the hair was exposed to sunlight for 2 weeks and buried in the soil for 2 months. Conclusions Although the exposure to sunlight and storage in soil for long times made drug-distribution analysis difficult, MSA could be applied even to hair strands collected from corpses left in severe environments.

In postmortem examinations, the drug analysis of hair is effective for revealing drug-use history. Additionally, a method to estimate the day of death using hair was previously developed by analyzing a single hair strand segmented at 0.4-mm intervals (micro-segmental hair analysis). However, for drowned bodies, drugs in the hair may be washed out due to soaking in water for extended periods. To evaluate the possibility of measuring drug distribution in the hair of drowned bodies, drug stability in hair samples soaked in various aqueous solutions was examined. First, reference hair strands of drug users containing specific drugs consistently along the hair shaft were prepared. The participants ingested 4 hay-fever medicines (fexofenadine, epinastine, cetirizine, and loratadine) every day for approximately 4 months before hair collection. Each reference strand was divided into regions, and each region was soaked in different solutions containing various solutes for extended periods up to approximately 2 months. In solutions without divalent ions (Ca2+ and Mg2+), the drug content in the hair decreased up to approximately 5 % with increasing salt concentration and soaking time. However, the decreased drug content was negligible in solutions containing divalent ions, implying that the divalent ions prevented drugs contained in hair from washing out. As natural river and sea waters contain divalent ions, the drugs in hair were hardly washed out even when the hair was soaked for 2 months. Thus, it was concluded that drug-distribution measurements using micro-segmental analysis can also be applied to the hairs of drowned bodies.HighlightsDrug stabilities in hair soaked in various aqueous solutions were examined.Drug concentrations in hair decreased depending on solutes and soaking time.Divalent ions, such as Ca2+ and Mg2+, prevent drugs from being washed out.River and sea waters hardly affected the drug contents in hair.Micro-segmental analysis is effective even for hair of drowned bodies.

Purpose Cannabis is regulated in many countries, and cannabis products are diversifying, which can hinder identification. Here, we report the seizure of a powder sample with a cannabis-like odor in a spice bottle labeled “nutmeg” and identification of the sample by chemical testing and cannabis DNA testing. Methods The sample was observed under a microscope, extracted with methanol, and analyzed by gas chromatography–mass spectrometry (GC–MS). The chemical profile of the seized powder was compared with that of nutmeg samples. Gas chromatography–flame ionization detection was used to estimate the total Δ 9 -tetrahydrocannabinol (Δ 9 -THC) concentration in the sample. A commercially available cannabis DNA testing kit was used to confirm the presence of cannabis plant DNA in the seized sample. Results The characteristics of cannabis in the seized powder were difficult to determine through microscopic observation alone. GC–MS analysis identified β-caryophyllene (an aromatic component of cannabis) and five cannabinoids unique to cannabis, including Δ 9 -THC. No common compounds were identified in the seized powder or nutmeg samples. The total Δ 9 -THC concentration in the sample was very high (approximately 47% by weight). Cannabis DNA testing confirmed that the seized powder contained cannabis. Conclusions The seized powder was found to be a processed product made from a finely pulverized resin-like cannabis concentrate. Our results indicate that combined chemical and DNA analysis should help identify cannabis-related samples in various forms.

[Display omitted] •Chiral SFC method for ephedrine and its stereoisomers was developed.•The method was suitable for crystalline methamphetamine including ephedrines.•Fast analysis (11min) with baseline separation was achieved.•Unsupervised multivariate analysis objectively classified seized methamphetamine. In forensic science, drug profiling is clarifying the identity of seized drugs of abuse based on their physicochemical properties and it is applied to various drugs, including crystalline methamphetamine. Impurity analysis is particularly important in drug profiling because the impurities can be a measure for speculating how the methamphetamine was synthesized in the clandestine laboratories. However, developments in scientific techniques have allowed the synthesis of high-purity, homogeneous crystalline methamphetamine, and thus new techniques to characterize methamphetamine are needed. In this study, we developed a method for chiral separation of ephedrine and its stereoisomers by supercritical fluid chromatography. Ephedrine is a common starting compound for methamphetamine synthesis. It possesses two chiral center carbon atoms and has four stereoisomers, (1R,2S)–(−)–ephedrine, (1S,2R)–(+)–ephedrine, (1S,2S)–(+)–pseudoephedrine, and (1R,2R)–(−)–pseudoephedrine. Because the stereostructure of ephedrines contained in methamphetamine seizure reflects the starting materials and the synthetic pathways, the stereoisomer ratio will provide additional information for drug profiling. The developed method achieved rapid separation of four isomers in about 11min with low limits of detection (1pg on column). Due to a switching valve connecting a chromatograph to a mass spectrometer, dense methamphetamine sample solutions containing small amount of ephedrines could be analyzed directly with a simple pre-treatment. Using multivariate analysis, 44 real samples were objectively grouped based on stereoisomer ratio. Our method is expected to improve the profiling of crystalline methamphetamine.

Purpose Drug distribution in scalp hair can provide historical information about drug use, such as the date and frequency of drug ingestion. We previously developed micro-segmental hair analysis, which visualizes drug distribution at 0.4-mm intervals in individual hairs. The present study examines whether the distribution profiles of drugs can be markers for the administration or external contamination of the drugs using scalp, axillary, and pubic hairs. Methods A single dose of anti-itch ointment containing diphenhydramine (DP) and lidocaine (LD) was topically applied to the axillary or pubic areas of two volunteers; DP was also orally administered; and LD was intra-gingivally injected. Scalp, axillary, and pubic hairs were assessed using our micro-segmental analysis. Results The localization of DP and LD differed within individual scalp hair strands, implying DP and LD were predominantly incorporated into scalp hair via the bloodstream and via sweat/sebum, respectively, showing double-peak profiles. However, DP and LD were distributed along the shafts of axillary and pubic hairs without appearance of the double-peak profiles when the ointment had been applied to the axillary and pubic areas. The distributions of DP and LD in scalp hairs did not significantly differ according to administration routes, such as oral administration, gingival injection, and topical application. Conclusions Micro-segmental analysis revealed differences in the distribution profiles of drugs in hairs, and distinguished hairs with and without external contamination. These findings will be useful for understanding of the mechanism of drug uptake into hair and for estimating the circumstances for a drug use.

Purpose Hair analysis can provide effective information to prove drug-facilitated crimes (DFCs). Herein, an analytical procedure for obtaining evidence of DFCs stronger than with conventional segmental hair analysis is demonstrated for an actual case. A victim reported to the police that, approximately 1 month earlier, she had consumed a drink, fallen asleep, and then been assaulted. Methods Her hair strands were collected to examine whether drugs were detected from her hair. Drug screening by liquid chromatography–high-resolution mass spectrometry (LC–HR-MS) revealed a specific peak, derived from zolpidem, on the chromatogram obtained from the hair extract. Micro-segmental analysis using an internal temporal marker (ITM) was performed to estimate the day of zolpidem ingestion using sensitive LC–low-resolution tandem mass spectrometry (MS/MS). The victim ingested cold medicine as an ITM twice, with an interval of 21.0 days, to calculate the actual growth rate of her hair. Her hair strands were collected again 2 weeks after the second ITM ingestion. A hair strand was cut at 0.4-mm intervals, and the distribution curves of zolpidem and the ITM in a hair strand were plotted. Results The estimated day of zolpidem ingestion was consistent with the day of the incident that she had reported. The two-step hair analysis proved that she had ingested zolpidem on the day of the incident. Conclusions The combination of drug screening by LC–HR-MS and determination of the day of drug ingestion using micro-segmental analysis by sensitive LC–MS/MS would be useful for elucidating the relationship between the drug and the incident when investigating DFCs.

Purpose Various forms of cannabidiol (CBD)-containing products are sold in Japan. CBD is easily converted to mixtures of ∆ 9 -tetrahydrocannabinol (∆ 9 -THC) and its isomer, ∆ 8 -THC, using household chemicals like diluted hydrochloric acid. This ease of production increases concerns regarding production of homemade THC mixtures. It is difficult to separate ∆ 9 -THC, ∆ 8 -THC, and CBD using thin-layer chromatography (TLC) on conventional silica gel. The selectivity of TLC on silver nitrate-impregnated silica gel (AgNO 3 -silica gel) differs from that of conventional silica gel. This study thus aimed to evaluate the separation ability of AgNO 3 -silica gel TLC. Methods To evaluate potential separation ability, standards of five THC isomers (∆ 9 -THC, ∆ 8 -THC, a pair of diastereomers of ∆ 10 -THC, and ∆ 6a,10a -THC), CBD, CBN, and ∆ 9 -THCA were analyzed by 10% AgNO 3 -silica gel TLC (developed using toluene, system A) and silica gel TLC [developed using n -hexane/diethyl ether (8:2, v/v), system B]. Then, mock homemade THC mixtures, prepared by heating crystalline CBD in acidic ethanol, were analyzed using systems A and B. Results System A showed clear separation between the five THC isomers and between ∆ 9 -THC, ∆ 8 -THC, CBD, and their by-products in the mock homemade THC mixture. However, system B did not separate some combinations of THC isomers and gave a single group-like spot to the THC mixture. Conclusion AgNO 3 -silica gel TLC shows high separation ability between THC isomers and among ∆ 9 -THC, ∆ 8 -THC, and CBD. It will thus be useful for analyzing homemade THC mixtures.