The application of time-of-flight secondary ion mass spectrometry (TOF-SIMS) for the characterisation of gunshot residue (GSR) from 0.22 caliber rimfire ammunition is reported. Results obtained by TOF-SIMS were compared with conventional scanning electron microscopy (SEM) studies. As could be expected, TOF-SIMS exhibited greater elemental sensitivity than SEM equipped with energy dispersive X-ray detection (SEM-EDX), and was also capable of detecting fragments characteristic of inorganic compounds. This preliminary study indicates that TOF-SIMS offers substantial potential for forensic GSR examinations as a complementary technique to SEM-EDX. In addition TOF-SIMS is applicable to the analysis of individual particles in the typical size range encountered in GSR casework.
Chemical etching, which is the most sensitive method to recover obliterated serial numbers on metal surfaces, has been practised quite successfully in forensic science laboratories all over the world. A large number of etchants suitable for particular metal surfaces based on empirical studies is available in the literature. This article reviews the sensitivity and efficacy of some popular etchants for recovering obliterated marks on medium carbon steel (0.31% C with ferrite-pearlite microstructure) used in automobile parts. The experiments involved engraving these carbon steel plates with some alphanumeric characters using a computer controlled machine "Gravograph" and erasing them to several depths below the bottom of their engraving depth. Seven metallographic reagents of which most of them were copper containing compounds were chosen for etching. The erased plates were etched with every one of these etchants using swabbing method. The results have revealed that Fry's reagent comprising cupric chloride 90 g, hydrochloric acid 120 mL and water 100mL provided the necessary contrast and was concluded to be the most sensitive. The same reagent was recommended by earlier workers for revealing strain lines in steel surfaces. Earlier, another reagent containing 5 g copper sulphate, 60 mL water, 30 mL (conc.) ammonium hydroxide, and 60 mL (conc.) hydrochloric acid was proved to be more sensitive to restore erased marks on low carbon steel (0.1% C with ferrite-pearlite structure) [M.A.M. Zaili, R. Kuppuswamy, H. Harun, Restoration of engraved marks on steel surfaces by etching technique, Forensic Sci. Int. 171 (2007) 27-32]. Thus the sensitivity of the etching reagent on steel surfaces appeared to be dependent on the content of carbon in the steel.
Classification of seized methamphetamine by impurity profiling can provide very useful information in criminal investigations of drug traffic routes, sources of supply and relationships between seizures. The aim of this study is to improve and develop an analytical method for detecting impurities such as starting materials and by-products in illegally prepared methamphetamine.HCl samples. A 50mg sample of methamphetamine.HCl was dissolved in 1 ml of buffer solution (four parts 0.1M phosphate buffer pH 7.0 and one part 10% Na2CO3). Impurities were extracted with 0.5 ml of ethyl acetate containing four internal standards (ISs) (n-decane, n-pentadecane, n-nonadecane and n-hexacosane) and analyzed by gas chromatography (GC) using a flame ionization detector (FID) on a DB-5 capillary column (0.32 mmi.d. x 30 m, film thickness 1.0 microm). The use of a middle-bore column offered better separation of the impurity peaks. The correction of the retention times of impurity peaks with four ISs made peak identification very accurate for subsequent data processing. Twenty-four characteristic peaks were selected for comparison and similarity and/or dissimilarity between samples, and the data were evaluated by the Euclidean distance of the relative peak areas after logarithmic transformation. The results indicate that the present method would be useful for methamphetamine impurity profiling.
The aim of this study was to evaluate the characteristics of traffic offenders with unusually high blood-alcohol concentrations (BAC>0.4g%) when arrested. The BAC that kills one person might be easily tolerated by another, depending on, among other things, the person's age, pattern of drinking, and the development of tolerance. The archives of two forensic laboratories, one in Sweden and the other in Wisconsin (USA), were searched to find traffic offenders with BACs>0.4g%. The results were compared in relation to the person's age and gender, mean BAC and the weekday and time of day of the arrest. The mean age (±standard deviation) of N=158 Swedish offenders was 45±9.0y, which was not significantly different from the 43±9.4y in N=233 Wisconsin drivers (p>0.05). Overall there were more men (78%) than women (22%) arrested with BAC's>0.4g%, although the proportion of women in Wisconsin (35%) was higher than in Sweden (9%) (p<0.001). The mean (median) and highest BAC did not differ between jurisdictions; 0.429g% (0.422) and 0.546g% in Sweden and 0.428g% (0.421g%) and 0.526g% in Wisconsin. In Sweden 40% of the arrests occurred on Fridays and Saturdays, whereas in Wisconsin the arrests of people with such high BAC's were more evenly distributed throughout the week. Forty eight percent of the arrests in Sweden were made between 12 noon and 6pm compared with 37% in Wisconsin. Neither the mean age of offenders nor their mean BAC seemed to depend on the weekday or time of day of the arrest. Attempting to drive with a BAC above 0.4g% verifies the development of an appreciable tolerance to ethanol-induced cognitive and psychomotor impairment. Reaching such a high BAC probably requires continuous heavy drinking over several days as opposed to an evening's binge drinking.
Due to their cannabis-like effects, synthetic cannabinoids have attracted much public attention since 2008. Thus, elucidation of the metabolic pattern and the detection of the intake of these drugs have been of major concern. In order to suggest appropriate urinary biomarkers to prove JWH-018 or JWH-073 intake, we selected the major metabolites of JWH-018 and JWH-073, namely (ω)-, (ω-1)-hydroxy, carboxy and 6-hydroxyindole metabolites, and validated a method for the quantification of these metabolites using solid-phase extraction based on LC-MS/MS analysis. Authentic urine specimens obtained from drug offenders were screened via a synthetic cannabinoid ELISA kit and were analyzed by LC-MS/MS for confirmation. Twenty-one out of a total of 52 samples (40%) were found positive for at least one metabolite of JWH-018 or JWH-073. N-pentyl hydroxy metabolites of JWH-018 and carboxy metabolites of JWH-018 and JWH-073 were detected in all positive samples. However, the rest of the metabolites were either not detected or only a small amount of them were found. A considerable variation was observed in the concentration ratio of (ω) and (ω-1)-hydroxy metabolites of JWH-018. Based on the results, it may have some pitfalls to determine the ingestion of specific synthetic cannabinoids by detecting a few metabolites, considering the continuous emergence of structurally related synthetic cannabinoids. Thus, use of synthetic cannabinoids should be proven carefully through comprehensive investigation of analytical results of biological specimens.
JWH-018 (1-pentyl-3-(1-naphthoyl)indole) is one of numerous potential aminoalkylindoles contained in products marketed as 'K2' or 'Spice'. Investigation of the urinary metabolites from consumption of these compounds is important because they are banned in the United States and many European countries. An efficient extraction procedure and gas chromatography-mass spectrometry (GC-MS) method were developed for detection of 'K2' metabolites in urine from individuals suspected of using these products. Analytical standards were used to elucidate the structure-specific mass spectral fragmentations and retention properties to confirm proposed identifications and support quantitative studies. A procedure for the synthesis of one of these metabolites (5-hydroxypentyl JWH-018) was also developed. Results are comparable to existing LC-MS/MS methods, with the same primary metabolites detected. The specific metabolite hydrolysis products include 4-hydroxpentyl, 5-hydroxypentyl, and N-pentanoic acid derivatives.
The disposition in mice of the cannabimimetics JWH-018 and JWH-073 in blood and brain following inhalation of the smoke from the herbal incense product (HIP) "Magic Gold" containing 3.6% JWH-018, 5.7% JWH-073 and less than 0.1% JWH-398 (w/w) is presented. Specimens were analyzed by HPLC/MS/MS. The validation of the method is also presented. Five C57BL6 mice were sacrificed 20 min after exposure to the smoke of 200 mg of "Magic Gold" and a second set of five exposed mice were sacrificed after 20 h. Twenty minutes after exposure to "Magic Gold" smoke, blood concentrations of JWH-018 ranged from 42 to 160 ng/mL (mean: 88 ng/mL ± 42) and those of JWH-073 ranged from 67 to 244 ng/mL (mean: 134 ng/mL ± 62). Brain concentrations 20 min after exposure to "Magic Gold" smoke for JWH-018 ranged from 225 to 453 ng/g (mean: 317 ng/g ± 81) and those of JWH-073 ranged from 412 to 873 ng/g (mean: 584 ng/g ± 163). Twenty hours after exposure to "Magic Gold" smoke, JWH-018 was detected and quantified in only two of the five blood samples. Blood concentrations of JWH-018 were 3.4 ng/mL and 9.4 ng/mL. JWH-073 was detected in only one blood specimen 20 h after exposure at 4.3 ng/mL. Brain concentrations 20 h post exposure for JWH-018 ranged from 7 to 32 ng/g (mean: 19 ng/g ± 9). JWH-073 was not detected in 20 h post exposure brain specimens. JWH-398 was not detected in any of the blood or brain samples. The disposition data presented with the limited data available from human experience provide reasonable expectations for forensic toxicologists in JWH-018 or JWH-073 cases. As with THC after smoking marijuana, blood and brain concentrations of JWH-018 and JWH-073 after HIP smoking can be expected to rise initially to readily detected values, and then drop dramatically over the next few hours to several ng/mL or ng/g, and finally to be at extremely low or undetectable concentrations by 24h apparently due to extensive biotransformation, and redistribution to body fat.
In this work, methods for the rapid identification, extraction, and quantification of the synthetic cannabinoid, JWH-018, from commercially available "Spice" (a herbal marijuana alternative) are presented. JWH-018 was identified in three different products using time-of-flight (TOF) mass spectrometry coupled with a direct analysis in real time (DART) ionization source, a process that was completed in less then five minutes and required no sample preparation. Extraction of the JWH-018 from the spice samples using an automated accelerated solvent extraction (ASE) instrument provided clean extracts with few plant pigments. Subsequent quantification by isocratic HPLC produced the following results (mg JWH-018/g plant material): Weekend Warrior brand "Hash": 90 (±3%)mg/g, Weekend Warrior brand "Leaf": 29 (±6%)mg/g, TrainWreck Hayze brand: 28 (±4%)mg/g. Vegetative samples spiked with JWH-018 gave a recovery of 97% (±1%).
Smoking mixtures containing the cannabimimetic indoles may still be available over-the-counter in several countries. Due to the high affinity of these compounds to the cannabinoid receptors, their effective dose is lower than that of the marijuana products resulting in a low concentration of the excreted metabolites accompanied by a higher psychoactive potency. Up to now the in vivo metabolism of the cannabimimetic indoles seems to be insufficiently investigated and no data have been published on an assay of JWH-018 in urine. In this publication the urinary metabolites of JWH-018 are reported. Using gas and liquid chromatography combined with tandem mass spectrometry two main monohydroxylated metabolites were identified in the forensic urine samples. Based on the differences in their electron ionization MS/MS spectra it is supposed that one is formed by hydroxylation of the indole ring whilst the other by hydroxylation of the N-alkyl chain. The main metabolites are almost completely glucuroconjugated, whereas minor ones (N-despentyl hydroxy-, carboxy-, dihydroxy-, and reduced di- and trihydroxy metabolites) were also present in the free fraction. The parent compound was not detected in urine.
Herbal smoking blends, available on the German market were analyzed and several known synthetic cannabinoids were identified (JWH-122 and JWH-018). In addition, we isolated a new active ingredient by silica gel column chromatography and elucidated the structure by nuclear magnetic resonance (NMR) methods. The compound was identified as JWH-307, a synthetic cannabinoid of the phenyl-pyrrole subclass with known in vitro binding affinities for cannabinoid receptors. To date, this is the first appearance of this subclass of cannabimimetics in such products. JWH-307 has been further characterized by gas chromatography accurate mass spectrometry (GC-HRMS), electrospray tandem mass spectrometry (ESI-MS/MS), ultraviolet (UV) and infrared (IR) spectroscopy. JWH-018 was among the first compounds banned by many countries world-wide including Germany. The identification of JWH-018 was striking, since this is the first report where JWH-018 recurred on the German market thus violating existing laws. A generic method was established to quantify synthetic cannabinoids in herbal smoking blends. Quantification was achieved using an isotopically labeled standard (JWH-018-D(3)). JWH-018 was found at a level of 150 mg/g while JWH-122 and JWH-307 occurred as a mixture at a total level of 232 mg/g.
We report the results of the Spanish and Portuguese working group (GEP) of the International Society for Forensic Genetics (ISFG) Collaborative Exercise 2002-2003 on mitochondrial DNA (mtDNA) analysis. Six different samples were submitted to the participating laboratories: four blood stains (M1-M2-M3-M4), one mixture blood sample (M5), and two hair shaft fragments (M6). Most of the labs reported consensus results for the blood stains, slightly improving the results of previous collaborative exercises. Although hair shaft analysis is still carried out by a small number of laboratories, this analysis yielded a high rate of success. On the contrary, the analysis of the mixture blood stain (M5) yielded a lower rate of success; in spite of this, the whole results on M5 typing demonstrated the suitability of mtDNA analysis in mixture samples. We have found that edition errors are among the most common mistakes reported by the different labs. In addition, we have detected contamination events as well as other minor problems, i.e. lack of standarization in nomenclature for punctual and length heteroplasmies, and indels. In the present edition of the GEP-ISFG exercise we have paid special attention to the visual phylogenetic inspection for detecting common sequencing errors.
Allele frequencies for 09 STR autosomal loci (D3S1358, D5S818, D7S820, D8S1179, D13S317, D18S51, D21S11, FGA and VWA) included in the AmpFlSTR Profiler Plus were obtained from a sample of unrelated individuals from Rio Grande do Sul (southern Brazil).
Spray cleaner is a cleaning product containing compressed 1,1-difluoroethane (HFC-152a) to blow dust off electric devices and other sensitive equipment; however, it is also inhaled to induce euphoria. This report describes three cases of death involving HFC-152a inhalation with spray cleaner under different circumstances. In case 1, death was during inhalation for euphoria with which led to having frostbite. In case 2, death may have been associated with suicidal intention. Case 3 was also considered an accidental autoerotic death. In all three cases, HFC-152a was detected at 99.2-136.2mg/l in blood samples, 94.5-191.9 mg/l in urine samples and 3.6-18.4 mg in the gastric contents according to gas chromatography with flame ionization detection. To prevent death associated with HFC-152a inhalation from spray cleaner, the danger of the sudden death should be announced to people, given the ready availability of commercial products containing HFC-152a.
A 13-year-old male was found dead in the woods subsequent to 1,1,1-trichloroethane (TCE) inhalation. Autopsy findings included tissue congestion of lung, liver and kidney. Certain precautions were taken in collecting and storing biological samples in order to prevent loss of TCE by evaporation. The availability of volatile solvents coupled with the increase of volatile substance abuse makes it easy for abusers to obtain.
A fatal case of 1,1,1-trichloroethane (methyl chloroform) poisoning, in which the patient survived, without recovering consciousness, for more than 3 years, is described. The brain showed symmetrical infarction of the lenticular nuclei and of the occipital cortex, changes which may have been the cause of neurological manifestations during life. The pattern of cerebral hypoxia was similar to, but not identical with that found in carbon monoxide poisoning, and might be specific for 1,1,1-trichloroethane poisoning.
Anecdotal evidence from forensic practitioners and studies conducted under controlled conditions have indicated that the reaction between 1,2-indanedione and the amino acids present in latent fingermark deposits is highly susceptible to ambient humidity. The addition of catalytic amounts of zinc chloride to the 1,2-indanedione working solution--usually in the order of 1:25 to 1:4 molar ratio (indanedione:zinc)--significantly improves the colour and luminescence of fingermarks treated under dry conditions but appears to have a negligible effect on fingermarks treated in humid environments. The results presented in this paper confirmed that zinc(II) ions added to the 1,2-indanedione working solution act as a Lewis acid catalyst, stabilising a key intermediate during a rate-limiting hydrolysis step. Furthermore, studying the reaction using a chromatography-grade cellulose substrate method previously reported confirmed that cellulose substrates play a major role in facilitating the indanedione-amino acid reaction by acting as a surface catalyst in the early stages of the reaction and by directing the formation of the desired luminescent product (Joullié's Pink).
This paper describes the spectroscopic study of the new fingerprint reagent, 1,2-indandione, using nuclear magnetic resonance spectroscopy (NMR) and mass spectrometry (MS). When 1,2-indandione is dissolved in methanol, NMR and MS show formation of a hemiketal similar to that proposed for DFO when it is dissolved in methanol. In contrast to DFO where reactivity with amino acids appears to be enhanced by hemiketal formation with alcohol solvents, the reactivity of 1,2-indandione towards amino acids is diminished by hemiketal formation. Alcohols should be avoided in 1,2-indandione formulations.
The reaction products of 1,2-indanedione (a new fluorescent fingerprint reagent) with glycine in methanol, at room temperature have been studied using excitation and emission and time-resolved fluorescence spectroscopy. Gas chromatography-mass spectroscopy (GC/MS) has also been used to determine which compounds are formed. Reaction products were identified using GC/MS as 2-carboxymethyliminoindanone (MW=203 g) and 1,2-di(carboxymethylimino)indane (MW=260 g). Identified compounds show room temperature fluorescence lifetimes of tau(1)=7.69 ns and tau(2)=1.27 ns. It is not clear yet which compound is having fluorescence lifetime of 7.69 ns and which one is showing 1.27 ns.
1,2-Indanedione treated fingerprints deposited on two substrates (thermal and carbonless paper) were swabbed and tested to determine the effect of the chemical on PCR-STR DNA typing. Samples from 10 post-treatment intervals were analyzed. Two extraction methods, Chelex and Qiamp, were used to determine the effect of extraction procedure on the quality of the DNA profiles. The LCN DNA samples were concentrated using Microcon 100 and amplified using the Profiler Plus amplification kit. 1,2-Indanedione did not adversely affect the DNA profiles obtained from the treated fingerprints. Partial DNA profiles were obtained at all post-development time frames. Both extraction methods produced comparable profiles although more "drop-ins" were observed with the Qiamp method. More "drop-outs" occurred in the DNA profiles from samples deposited on the thermal substrate compared with carbonless substrate.
1,2-indanedione is an emerging fingermark reagent used on porous surfaces. The general consensus is that this reagent is at least as sensitive as DFO, with some research showing higher sensitivity for 1,2-indanedione as opposed to DFO. However, a number of discrepancies existed in the literature as to which formulation and which development procedure produces optimal results. This project set out to investigate the best formulation and development procedure under Australian conditions, encompassing all published recommendations as well as some novel approaches. 1,2-indanedione formulations were compared with respect to initial colour, fluorescence, concentration of reagent, acetic acid concentration, and the effect of different carrier solvents. Numerous development conditions were investigated, including a conventional oven, a heat press and humidity. Further enhancement using metal salt treatment and liquid nitrogen was also evaluated. The heat press set at 165 degrees C for 10s proved to give the best initial colour and most intense luminescence. Secondary metal salt treatment improved initial colour and luminescence. The Polilight, the VSC 2000, and the Condor Chemical Imaging macroscope have been used to detect the fingerprints developed with 1,2-indanedione on a variety of high- and low-quality porous and semi-porous surfaces, with impressive results overall. Laboratory and field tests were conducted to compare 1,2-indanedione with DFO and ninhydrin as well as to investigate the position of 1,2-indanedione in the sequence of reagents for fingermark detection on porous surfaces. Overall, 1,2-indanedione proved to be a viable alternative to traditional methods for the detection of fingermarks on porous surfaces, with more fingermarks being developed using this reagent on real samples than both DFO and ninhydrin and a combination of the two reagents.
The immunoglobulin allotypes G1m(1,2,3) and G3m(10,21) were typed in 2855 unrelated West German adult individuals. 1455 individuals were typed for the factors Km(1,3). Phenotype and haplotype frequencies are reported. The usefulness of this routine typing programme in paternity tests is demonstrated in three case reports.
The presence of Gm(1,2,4,10,21) and Km(1) factors in vitreous humor taken from human corpses was investigated. The results revealed a good agreement between the factors detected in this biological material and in blood. Their presence in vitreous humor is independent of the secretor type.
The photochemically induced fluorescence (PIF) studies of 1,3-diethyl-1,3-diphenylurea or ethyl centralite (EC) as stabilizer have been carried out under various conditions. Influences of solvent type (water, methanol, acetonitrile and chloroform), oxygen dependence and UV irradiation time on the spectroscopic properties of EC were studied. In order to obtain a better understanding of the photochemical mechanism, products were identified by mass spectrometry study. A novel fluorimetric method has been developed for the determination of EC based on the PIF. The method is based on the use of UV irradiation to produce fluorescent derivatives from EC as a non-fluorescent molecule. The determination is carried out by UV irradiation for 4min through measuring the fluorescence intensity in 354nm when an excitation wavelength of 227nm was used. Parameters related to the analytical signal and to the PIF are optimized. The linear range for determination of EC was 4×10(-8) to 2×10(-6)molL(-1) and the limit of detection (LOD) was 2×10(-8)molL(-1) with relative standard deviation (R.S.D.) of 3% (n=5). Finally, the proposed method was successfully applied for the determination of EC in real propellant samples and the acquired results were favorably compared to those obtained with HPLC method.
In 2008, the New Zealand Government passed an amendment to reschedule what were, at the time, the active ingredients of 'party pills' in New Zealand. Since then, submissions of tablets and powders to the Institute of Environmental Science and Research (ESR) Limited have included ingredients not previously seen among drug seizures in New Zealand. These new components, confirmed by the synthesis of standards, included some beta-ketone (βk) analogues of 3,4-methylenedioxyamphetamine (MDA). Though not yet seen in tablet or powder seizures, the synthesis and the analytical data for βk-DMBDB ((beta-ketone)-N,N-dimethyl-1-(1,3-benzodioxol-5-yl)-2-butanamine) are reported here for the first time.
The use of synthetic pharmaceuticals in phytotherapeutics can be defined as an illegal practice, since these compounds are normally present as non-declared compounds in the phytotherapeutical formulations. This work aims to show the development of an analytical method based on adsorptive cathodic stripping voltammetry (AdCSV) for the simultaneous determination of 1,4-benzodiazepines and amfepramone. The developed method was used to measure seven benzodiazepines (clonazepam, flurazepam, alprazolam, midazolam, medazepam, chlordiazepoxide, and diazepam) and amfepramone in slimming formulations that have been commercialized in Brazil. This method permits the screening of adulterant classes in a single voltammetric run by using a hanging mercury drop electrode as a working electrode and Ringer buffer (pH 10.0) as a supporting electrolyte. Recovery values ranging from 92.0% to 117.0% demonstrate the reliability of the method in the determination of adulterants in real samples. Among the 12 samples studied by the proposed method, 4 were demonstrated to be adulterated by 1,4-benzodiazepines.
A micellar electrokinetic chromatography (MEKC) method was optimised for simultaneous analysis of gamma-hydroxybutyric acid (GHB), gamma-butyrolactone (GBL), and 1,4-butanediol (BD). Best conditions for separation and baseline stability were achieved using a carrier electrolyte comprising 30.0mM sodium barbital and 150.0mM sodium dodecyl sulphate (SDS) at pH 10.2. Calibration functions were linear, giving correlation coefficients (r(2)) >0.998 for the three target compounds. Limits of detection (LOD) defined as three times the noise, were 5.1mg/l, 0.34 and 0.25g/l for GHB, GBL and BD, respectively. The repeatability of migration times and peak areas, expressed as the R.S.D. (n = 9) was better than 0.41 and 3.05%, respectively. Some casework samples were analysed using the optimised conditions.
We report a case of intoxication resulting from the ingestion of a liquid, sold in the illicit market as "liquid ecstasy," which was found to contain 1,4-butanediol, a metabolic precursor of gamma-hydroxybutiric acid (GHB). Identification of the substance in the liquid was performed by gas chromatography-mass spectrometry (GC-MS). The toxicological analysis of blood, urine and gastric content of the victim was performed by immunoassay and gas chromatography with nitrogen-phosphorus detection as screening techniques and by means of GC-MS for confirmation and quantitation of 1,4-butanediol and GHB. The following drug concentrations were found: 82 microg/ml (blood), 401 microg/ml (urine) and 7.4 microg/ml (gastric content) for 1,4-butanediol and 103 microg/ml (blood), 430.0 microg/ml (urine) for GHB. In addition to these, other drugs detected and their blood concentration found in this case were methylenedioxymethylamphetamine (MDMA) 0.23 microg/ml and its metabolite methylenedioxyphenylamphetamine (MDA) 0.10 microg/ml. In the urine, a concentration of 0.10 microg/ml of benzoylecgonine was also found.
Postmortem diagnosis of diabetes and a diabetic coma can be difficult because of the lack of characteristic morphological findings. 1,5-Anhydroglucitol (1,5-AG), the 1-deoxy form of glucose, competes with glucose for reabsorption in the kidneys. Therefore, diabetics with a permanent hyperglycemia show significantly lower serum concentrations of 1,5-AG than non-diabetics. A liquid chromatography-mass spectrometric method for the determination of 1,5-AG in serum and postmortem blood was developed and validated according to international guidelines. Linearity was given between 1 μg/ml and 50 μg/ml. Recovery rates ranged between 70.8% and 89.8%, the limit of quantification of the procedure was 0.20 μg/ml, limit of quantification was 0.55 μg/ml. Serum of 199 diabetics and 116 non-diabetics and femoral blood of 31 diabetic and 27 non-diabetic deceased was measured. Average concentrations were significantly (p<0.001) higher in non-diabetics compared to diabetics ante and postmortem. Seven of the diabetics may have died because of a hyperglycemic coma indicated by a sum formula of Traub>450 mg/dl. 1,5-AG average concentrations in these deceased were not significantly different to diabetics which did not die because of a diabetic coma. Concentrations of 1,5-AG give a hint for not well controlled diabetes antemortem and postmortem and can be assumed as an additional and alternative information postmortem to the measurement of HbA1c or fructosamine.
This paper describes the study of the reaction between 1, 8-diazafluoren-9-one (DFO) with the amino acid L-alanine in methyl alcohol. Particular interest was paid to the possible role of the solvent which appears to react with the DFO to form a hemiketal that is the reactive species. A potential reaction pathway is proposed based on the current data collected. The reaction intermediates and products were identified by a variety of spectroscopic methods including mass spectrometry (MS), nuclear magnetic resonance (NMR) spectroscopy, and X-ray crystallography.
As part of a European union (EU) support program in forensic science for the Palestinian police, a forensic assistance software was designed to respect the quality management of the anti-terrorism laboratory of the Palestinian police by the different forensic teams in the disconnected Palestinian cities. This tool not only proposes up-to-date detection and identification protocols for traces, explosives, drugs, GSR, biological samples, but also appeared to be a convenient support for forensic practice teaching.
The addition of negroid phenotypes to the already heterogeneous population of Israel caused us to reuse the enzymes G6PD and PGD which are known to have a better discrimination power in a negroid population than in caucasians. We have developed a system for combined phenotyping of G6PD and PGD. This system answers the requirements of the above enzymes and results in a negroid population than in caucasians. We have developed a system for combined phenotype-amount of sample and reagents needed and time spent.
Allele frequencies for the eight STRs included in the GenePrint PowerPlex 1.2 kit were obtained from three population groups that are resident in the United Arab Emirates (UAE); 228 unrelated UAE individuals, 194 unrelated Indian individuals and 197 unrelated Pakistani individuals were analysed.
Allele frequencies for 10 STRs including the GenePrint PowerPlex 1.2 loci and also D3S1358, HumvWA and HumFGA were obtained from a sample of unrelated individuals from El-Minia City.
A minisatellite probe, MZ 1.3, detecting hypervariable fragment patterns was isolated from a human genomic library. A repetitive sequence of 27 bp length was identified which is contained in the probe approx. 40 times. The MZ 1.3 repeat shows variable homology of 53-73% to the repetitive sequence of the protein III gene of the bacteriophage M13 genome. Polymorphic restriction fragment patterns were found with MZ 1.3 using the enzymes Hinf I, BstN I, Hae III, Mbo I, PstI/Pvu II, and Rsa I. An average of 18 polymorphic fragments was observed using Hinf I as enzyme. The band sharing frequency after Hinf I digestion among unrelated individuals was determined to be 23.8 +/- 7.2%. An example for the application of MZ 1.3 to paternity testing in an incest case is given. The probe can be used with radioactive or non-radioactive detection systems. An approach is presented to compare polymorphic fragment patterns from individuals obtained by independent gel runs on the basis of relative band positions (RBP) and calculated in a computerized analysis.
The aim of this study was to ascertain if a relationship between weapon choice and psychopathology existed. The perpetrators (103) were evaluated at the Department of Criminology and Forensic Psychiatry of the University of Bari in southern Italy. Psychiatric examination and psycho-diagnostic tests were administered for each of the perpetrators and a database was subsequently formulated. The results showed a significant correlation between some types of mental disorder and weapon choice. A strong correlation was found between delusional disorders and the use of sharp weapons, whereas depressive disorders were more strongly associated with asphyxia. Organic disorders were found to be highly correlated with the use of blunt instruments. In cases where the homicide was the result of an impulsive reaction, the use of sharp weapons was most often observed.
To determine the frequency and degree of milk aspiration in infant death cases, immunohistochemical examinations were performed on lung sections from 41 sudden death cases and 64 in-hospital death cases using anti-human alpha-lactalbumin antibody. Milk aspiration to some degree was detected in more than half of the sudden death cases and in about one-third of the in-hospital death cases. A semi-quantitative examination of the amount of aspirated milk was subsequently performed in the positive cases. The amount of aspirated milk in the sudden death cases was significantly higher than that in the in-hospital death cases. The frequency distribution of the amount of aspirated milk was similar in shape in both groups. In most cases, a very small amount of aspirated milk was detected. The aspirated milk was assumed to be a result of occasional gastroesophageal reflux or cardiopulmonary resuscitation. However, in five cases, much larger amounts of aspirated milk were found. In these cases, milk aspiration may have been an important part of the cause of death. We concluded that slight milk aspiration is not rare in infant death cases, and that in a few cases, the aspiration is lethal. An immunohistochemical screening test is available to perform a postmortem diagnosis in these cases.
A simple technique was employed for measurement of potassium loss (K(los)s) from normal and from postmortem rat erythrocytes during controlled exposure to physiologically isosmotic NaCl solution. Potassium loss from the cells decreased in a (non-linear) time-related manner during the 0-108 h postmortem period; expression of the data in the form of a double logarithmic plot (log K(loss) versus log postmortem interval (PMI) linearized the relationship between 18 and 108 h post mortem (r = -0.86; P less than 0.001 (n = 24)). Experimental data revealed that the observed postmortem changes in K(loss) were associated with and probably resulted from, the postmortem decrease in magnitude of the potassium concentration gradient across the erythrocyte membrane. Attention is drawn to the possibility of utilizing measurements of in vitro loss of potassium from erythrocytes as a means of estimating time elapsed since death.
Sudden infant death syndrome (SIDS) constitutes a considerable percentage of infant death of unknown etiology. The genetically controlled pathway of cytokine mediated response to inflammation is presumed to play a role in SIDS. The A allele of SNP -592 of the promoter region of the anti-inflammatory cytokine IL-10 has been suggested to be associated with SIDS. Herein we investigated whether we could confirm this finding by SNP genotyping a series of 123 cases of SIDS and 406 control cases. We did not find a correlation between the A allele or an A allele containing genotype of IL-10 promoter SNP -592 and SIDS which is in contrast to previous studies. Also, in concordance with previous work, no association of the A allele or A allele containing genotypes of IL-10 promoter SNP -1082 and SIDS was found.
Allelic frequencies, forensic parameters and admixture values for eleven STR loci (F13B, TPOX, CSF1PO, F13A01, D7S820, LPL, TH01, vWA, D13S317, FESFPS, and D16S539) were determined in a sample of unrelated individuals, European descendants from Rio de Janeiro area, Brazil.
The forensic value of Y-STR markers in Guiné-Bissau was accessed by typing of 215 males. Allele and haplotype frequencies, determined for loci DYS19, DYS389-I, DYS389-II, DYS390, DYS391, DYS392, DYS393, DYS437, DYS438, DYS439 and the duplicated locus DYS385, are within the limits of variation found in other populations south of the Sahara. The level of discrimination achieved is Guineans is higher than for European or other African populations with comparable data. The haplotype diversity of 0.9995 is reduced to 0.9981 when the minimal haplotype is considered thus revealing the importance of increasing the number of typed loci.
11-Nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid ethyl ester (THC-COOEt) can be presumed to be a mixed metabolite formed during combined consumption of cannabinoids and alcohol. In order to examine this hypothesis, THC-COOEt and its deuterated analogue D(3)-THC-COOEt were synthesized as reference substance and internal standard from the corresponding carboxylic acids and diazoethane and methods were developed for the sensitive detection of THC-COOEt in plasma and hair based on gas chromatography-electron impact mass spectrometry after silylation with N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI-MS) as well as tandem mass spectrometry (GC-NCI-MS-MS) after derivatization with pentafluoropropionyl anhydride. The methods were applied for THC-COOEt determination to plasma samples from 22 drunk driving cases which contained both ethanol (0.30-2.16 mg/g) and THC-COOH (15-252 ng/mL) as well as to 12 hair samples from drug fatalities which were both positive for THC (0.09-2.04 ng/mg) and fatty acid ethyl esters as markers of chronic alcohol abuse (0.70-6.3 ng/mg). In none of these samples THC-COOEt could be found with limits of detection of 0.3 ng/mL in plasma and 2 pg/mg in hair in 11 samples using GC-NCI-MS and 0.2 pg/mg in one sample using GC-NCI-MS. Therefore, the use of this compound as a marker for combined cannabis and alcohol consumption could not be achieved.
Allele and haplotype frequencies for the 12 Y-specific short tandem repeats (STR) loci DYS19, DYS385a/b, DYS389I/II, DYS390, DYS391, DYS392, DYS393, DYS437, DYS438, DYS439 (PowerPlex Y System STR Amplification Kit, Promega) were determined in a population sample of 187 unrelated China Han in northeast China.
Carbon monoxide (CO) poisoning as a cause of death is well documented in industrialized countries. The objective of this study was to compare demographic data in deaths due to accidents (in fires) and suicides in the same population between 1988 and 1998. Furthermore, the potential effect of a community wide education effort regarding safety in the home was assessed. Postmortem reports were reviewed for all deaths examined at the Office of the Cuyahoga County Coroner in Cleveland, OH, USA. During the study period, there were 209 accidental deaths due to fires in the home (6.5% of all accidents in the home) and 182 CO deaths by suicide (9.8% of all suicides). Demographic characteristics of the two groups differed: while males represented the majority of cases in both groups (55% of accidents, 70% suicides), race specific death rates were higher for whites than blacks (18/100,000 white, 3/100,000 black) in suicides compared with 29/100,000 deaths for blacks and 11/100,000 for whites in accidental cases. Fire deaths were prevalent in the young (0-9 years) and old (>60) whereas in the suicide group the age specific death rate was highest for those over 70 years. The majority of fire deaths occurred in the city of Cleveland but suicides were prevalent in the suburbs. More fire deaths occurred in December than any other month whereas more suicides occurred in April. In 1992, there was a community wide effort to provide free smoke detectors to residents in Cleveland. In 1992, there were 4.2/100,000 fire deaths in the city. This decreased to 0.6/100,000 in 1996, increased to 1.2/100,000 in 1997 followed by a decrease to 0.8/100,000 in 1998. This suggested that the program may have aided in decreasing these types of deaths. Deaths due to fires in the suburbs were <1/100,000 throughout the study period.
We have obtained Y-STR haplotypes in 12 loci (DYS19, DYS385, DYS389I, DYS389II, DYS390, DYS391, DYS392, DYS393, DYS437, DYS438 and DYS439) from 215 Buryat males. We have found that one haplotype (15-11,18-13-28-23-10-11-14-14-10-12) comprises more than 30% of Y chromosomes in this population while another haplotype (14-11,13-14-30-23-10-14-14-14-10-10) comprises additional 14% of chromosomes. The population under study seems to be very homogenous as far as Y chromosome is regarded and the most frequent haplotype seems to be the modal haplotype for Buryats.
In this study, the concentrations of 11-nor-Δ(9)-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in pubic, axillary and beard hair were measured and the correlation between the concentrations of THCCOOH in head and pubic hair from same cannabis users were evaluated. The papers on body hair analysis for THCCOOH were rarely found although police officers submit body hair as a complimentary specimen to forensic laboratories in case cannabis users had no hair. Head, pubic, axillary, and beard hair were collected. All hair samples were cut into 0.5mm segments and decontaminated with methanol, digested with 1 mL of 1M NaOH at 85 °C for 30 min and extracted in 2 mL of n-hexane:ethyl acetate (9:1) two times after adding 1 mL of 0.1N sodium acetate buffer (pH = 4.5) and 200 μL of acetic acid followed by derivatization with 50 μL of PFPA and 25 μL of PFPOH for 30 min at 70 °C. The extracts were analyzed using gas chromatography tandem mass spectrometry operating in negative chemical ionization mode (GC/MS/MS-NCI). We determined the concentrations of THCCOOH in both pubic and head hair. The concentrations of THCCOOH in pubic hair were higher than those in head hair. We also evaluated the concentrations of THCCOOH in body hair (pubic, axillary and beard hair) and head hair according to the positive/negative urine test results. There was no statistically significant difference in the concentrations of THCCOOH in head and body hair according to urine results.
In this study, we investigated the patterns of cannabis users (n=412) according to their sex, age, and the results of urinalysis and hair analysis, and classified the concentrations of THCCOOH in hair into three categories to examine the levels of cannabis use. We also compared the concentrations of THCCOOH in hair root, hair without the hair root and whole hair and examined the relationship among them according to the results of urinalysis. The hair samples were washed, digested with 1ml of 1M NaOH at 85°C for 30min and extracted with 2ml of n-hexane:ethyl acetate (9:1) two times after adding 1ml of 0.1N sodium acetate buffer (pH 4.5) and 200μl of acetic acid. The final mixture was derivatized with 50μl of PFPA and 25μl of PFPOH for 30min at 70°C. The solution was evaporated, and the residue was reconstituted in 40μl of ethyl acetate and transferred to an autosampler vial. One microlitre was injected into the GC/MS/MS-NCI system. The concentrations of THCCOOH ranged from 0.06 to 33.44pg/mg (mean 2.96; median 1.32) in hair from cannabis users who had positive urine results and ranged from 0.05 to 7.24pg/mg (mean 1.35; median 0.37) in hair from cannabis users who had negative urine results. The average concentration of THCCOOH in hair from cannabis users who had positive urine results was higher than that from cannabis users who had negative urine results. Male cannabis users in their forties were predominant. We classified the concentrations of THCCOOH in hair into three groups (low, medium and high), and could use the grouping of THCCOOH in hair as a guide for determining the level of use. The low, medium and high concentration ranges for THCCOOH in hair were 0.05-0.24, 0.25-2.60 and 2.63-33.44pg/mg, respectively. We also investigated 28 hair samples with the root. The highest concentrations of THCCOOH were seen in the hair root from 18 out of the 28 hair samples. The average concentrations of THCCOOH in hair root, hair without hair root and whole hair from cannabis users who had positive urine results were higher than those who had negative urine results.
