Evaluation of 5-(4-nitrophenyl)-2,4-pentadien-1-al (NPPD) as a tracer for shadowing pursuits

The chemical compound 5-(4-nitrophenyl)-2,4-pentadien-1-al (NPPD), called "spy dust," was used in the Soviet Union as a shadowing pursuit, the act of following someone secretly, for investigating the activities of diplomatic personnel. It is also useful for counter-terrorism, and some criminal cases in the forensic science field. In this paper, it was synthesized and evaluated as a tracer for shadowing pursuits. The method for utilizing this reagent was very simple: it was dissolved in methanol (1 mg/mL) and sprayed on the restricted area. If the suspect was to enter this area or touched the sprayed material, NPPD was attached to the suspect's shoe surface or hands. The color examination was a two-steps process: first was the addition of 1 mL of a 0.1% naphthoresorcinol methanol solution to the methanol extracts of a methanol-contained cotton swab used to smear some surfaces of the suspect, and second, the addition of 1 mL of concentrated hydrochloric acid, which turned the solution dark red. The gamma max of the colored solution was 510 nm, measured by ultraviolet-vis spectroscopy. Detection limits for three methods were determined: a visual method (detection limit 100 ng/3 mL), an ultraviolet-visible spectrometric method (detection limit 10 ng/3 mL), and a selected-ion-monitoring gas chromatographic/mass spectrometric method (detection limit 300 pg/injection). The forensic utility of NPPD was demonstrated for two simulated cases: a theft case and a case where NPPD was used as a tracer to prove that an automobile had entered a restricted area. These examinations prove NPPD is a useful shadowing pursuit (spy dust) for the forensic science field.     

Evaluation of the rapid analyte measurement platform (RAMP) for the detection of Bacillus anthracis at a crime scene

The aim of this study was to evaluate the accuracy and reliability of the rapid analyte measurement platform (RAMP) for presumptive identification of Bacillus anthracis spores. Test samples consisted of serial dilutions of spore preparations of several Bacillus species, including B. anthracis, which were tested, using the RAMP Anthrax test cartridge, according to the manufacturer's instructions. The fluorescence labelled antibody-antigen complexes were detected in the portable reader after 15 min following sample addition. Dilutions of common environmental and household powders were also tested to identify possible false positive results. B. anthracis spores were identified reliably in test samples containing more than 6000 spores. The test kits were highly specific, showing no cross reactivity with other Bacillus species or any environmental powders tested. The RAMP system for detection of B. anthracis spores, from environmental samples, showed consistent results under a variety of analytical conditions, enabling the trained user to provide a rapid, accurate preliminary risk assessment of a suspected bioterrorism incident.     

Identification of 1-butyl-3-(1-(4-methyl)naphthoyl)indole in a herbal mixture

Besides the cannabinoid mimetic JWH-073, a novel 4 methylnaphthoyl homologue of JWH-073 was detected in a herbal mixture. The structure of the compound was elucidated after thin layer chromatographic enrichment from the herbal mixture by nuclear magnetic resonance (NMR) and gas chromatographic mass spectrometric (GC-MS) analysis. The paper outlines data after GC-MS, liquid chromatography mass spectrometry (LC-MS) and NMR spectroscopy, and describes the structure elucidation.     

Separation and structural characterization of the synthetic cannabinoids JWH-412 and 1-[(5-fluoropentyl)-1H-indol-3yl]-(4-methylnaphthalen-1-yl)methanone using GC-MS, NMR analysis and a flash chromatography system

The 'herbal highs' market continues to boom. The added synthetic cannabinoids are often exchanged for another one with a high frequency to stay at least one step ahead of legal restrictions. While most of these substances were synthesized for pharmaceutical purposes and have been described in the scientific literature before, others originate from clandestine laboratories supplying this lucrative market. In this paper, the identification and structure elucidation of two synthetic cannabinoids is reported. The first compound, 1-[(5-fluoropentyl)-1H-indol-3yl]-(4-methylnaphthalen-1-yl)methanone, was found along with AM-2201 in a 'herbal mixture' obtained via the Internet. For isolation of the substance from the mixture, a newly developed flash chromatography method was used providing an inexpensive and fast way to gain pure reference substances from 'Spice' products for the timely development or enhancement of analytical methods in the forensic field. The second substance, 4-fluoronaphthalen-1-yl-(1-pentylindol-3-yl)methanone (JWH-412) was seized by German authorities as microcrystalline powder, making it very likely that it will be found in 'herbal mixtures' soon.     

高效液相色谱法测定人血清中安眠酮及其苯甲基羟化代谢物的浓度

本文建立了用反相高效液相色谱法(RP-HPLC)测定人血清中安眠酮及其苯甲基羟化代谢物-2-甲基-3[2-(羟甲基)-苯基]-4(3H)喹唑酮(Ⅰ)的浓度。安眠酮浓度在1-35μg/ml范围内呈直线相关(相关系数r=0.9980;回归方程y=0.06324x—0.1029),方法回收率平均为102.08±9.987(SD)％(n=5),检出限为1ng。其代谢物Ⅰ按原型安眠酮的线性浓度测定其相对量。本法为测定中毒者体内安眠酮及其代谢物Ⅰ的血浓度提供可行的手段。     

Km(3) identification by enzyme-linked immunosorbent assay (ELISA) as an internal control for Km(1) activity determined by inhibition in dried bloodstains

A stability study comparing the identification of kappa marker Km(1), using the classical inhibition of agglutination, and the identification of Km(3), using an automated enzyme-linked immunosorbent assay (ELISA) technique, was done. Preliminary tests were performed to establish the specificity and sensitivity of the methods. Based on the results, the quantities of stain required to detect each marker were determined. Blood samples from 24 staff donors of known phenotype were aged at room temperature and at 37 degrees C in the dried stain and liquid forms. In addition, 192 stains from cases 1 to 7 months old and 76 staff-donor stains from 1 1/2 to 10 years old were tested in dried stain form. The known sensitivity of the ELISA technique was exploited by deliverately testing a decreased quantity of antigen. As control stains were aged beyond the detectable limits of sensitivity, results consistently showed an almost simultaneous success or failure to detect Km(1) and Km(3). This indicates that the interpretive criteria established for ELISA are sufficiently demanding to eliminate the danger of reporting false Km(-1) results but true Km(3) results.     

Identification of 2‐(ethylamino)‐1‐(4‐methylphenyl)‐1‐pentanone (4‐MEAP), a New “Legal High” Sold by an Internet Vendor as 4‐Methyl Pentedrone

Online vendors are offering a new legal high, 4‐methylpentedrone (4‐MPD). Information for potential users provided by internet vendors of 4‐MPD includes incorrect structures and nonexistent CAS numbers. A sample of 4‐MPD was obtained and analyzed using GC‐MS, NMR, and LC‐EIS. The fragmentation data from the GC‐MS and LC‐EIS produced an M‐1 ion that suggested the molecular mass was 219 amu, rather than 205 amu as calculated for 4‐methylpentedrone. The difference in molecular mass corresponded to the addition of a methyl group. Based on the mass and fragmentation pattern, two standards were synthesized, 2‐(ethylamino)‐1‐(4‐methylphenyl)‐1‐pentanone and 1‐(4‐methylphenyl)‐2‐(propylamino)‐1‐butanone. The synthesis involved bromination of the appropriate ketone followed by the reaction with ethylamine or propylamine. Based on the NMR data and unique fragmentation patterns produced by these molecules, the sample was identified as 2‐(ethylamino)‐1‐(4‐methylphenyl)‐1‐pentanone, not 4‐methylpentedrone.     

Detection of significant gender differences by odontometry as illustrated by a representative group from Lebanese (East-Mediterranean) population

This study was conducted on a sample of the Lebanese population. Its aim was to verify differences in dental dimensions between the genders as was found by other authors in other populations. It is concluded that gender dental differences constitute an additional important, though not-decisive element, in identification of courpses.     

A distinct Y-STR haplotype for Amelogenin negative males characterized by a large Y(p)11.2 (DYS458-MSY1-AMEL-Y) deletion

The use of STR multiplexes with the incorporated gender marker Amelogenin is common practice in forensic DNA analysis. However, when a known male sample shows a dropout of the Amelogenin Y-allele, the STR system falsely genotypes it as a female. To date, our laboratory has observed 18 such cases: 12 from our Y-STR database and six from casework. A study on 980 male individuals in the Malaysian population using the AmpFlSTR Y-filer has revealed a distinct Y-chromosome haplotype associated with the Amelogenin nulls. Our results showed that whilst the Amelogenin nulls were noticeably absent among the Chinese, both the Indians and Malays exhibited such mutations at 3.2 and 0.6%, respectively. It was also found that the Amelogenin negative individuals predominantly belonged to the J2e lineage, suggesting the possibility of a common ancestor for at least some of these chromosomes. The null frequencies showed concordance with the data published in Chang et al. [Higher failures of Amelogenin sex test in an Indian population group, J. Forensic Sci. 48 (2003) 1309-1313] on a smaller Malaysian population of 338 males which used a Y-STR triplex. In the current study, apart from the absence of the Amelogenin Y-locus, a complete absence of the DYS458 locus in all the nulls was also observed. This study together with the 2003 study has indicated a similar deletion region exists on the Y(p)11.2 band in all the 18 Y-chromosomes. Using bioinformatics, this deletion has been mapped to a region of at least 1.13 Mb on the Y(p)11.2 encompassing the Amelogenin, MSY1 minisatellite and DYS458 locus. Further, the Y-filer haplotypes revealed an additional null at Y-GATA H4 in two of the Indian males presented here.