微波消解ICP-MS法测定人头发中24种元素的含量

目的建立人头发中24种无机元素的电感耦合等离子体质谱（inductively coupled plasma-mass spec-trometry,ICP-MS）分析方法。方法采用微波消解法处理样品,以铟（115In）作内标,用ICP-MS分析人头发中的24种元素含量。同时检测56例健康志愿者和10例海洛因滥用者头发中24种元素含量。结果 24种元素的方法检出限范围为0.0003~10.14μg/g,标准物质的测得值与标准值基本相符。海洛因滥用者经戒毒治疗后头发中镁、镓、钡含量下降。结论该方法灵敏度、准确度高,适用于头发中24种元素的测定。     

A fatal dichlorvos poisoning: concentrations in biological specimens

Abstract:  A 54-year-old man was found dead with a bottle containing a brownish fluid near him. A toxicological screening was carried out in blood, urine, and stomach content. Only dichlorvos (2,2 dichlorovinyl O-O dimethylphosphate or DDVP) was found. A simple and rapid method, using DDVP-D₆ as an internal standard, was developed for the determination of DDVP by gas chromatography/mass spectrometry (GC/MS). The method was linear from 1 to 10 mg/L. Intraday and interday precisions were all <15%. DDVP concentration in cardiac blood was approximately four times higher than in peripheral blood. A high concentration was found in the heart showing a cardiac tropism of DDVP, kidney and lung concentrations being much lower. No DDVP was found in liver. DDVP stomach content was 38 g. The amount presumed ingested was 82 g, c . 1000 mg/kg of body. The oral LD₅₀ for DDVP ranges between 20 and 1090 mg/kg in animals but is not known for humans.     

Average Probability that a "Cold Hit" in a DNA Database Search Results in an Erroneous Attribution

Abstract:  We consider a hypothetical series of cases in which the DNA profile of a crime-scene sample is found to match a known profile in a DNA database (i.e., a "cold hit"), resulting in the identification of a suspect based only on genetic evidence. We show that the average probability that there is another person in the population whose profile matches the crime-scene sample but who is not in the database is approximately 2( N  −  d ) p _A , where N is the number of individuals in the population, d is the number of profiles in the database, and p _A is the average match probability (AMP) for the population. The AMP is estimated by computing the average of the probabilities that two individuals in the population have the same profile. We show further that if a priori each individual in the population is equally likely to have left the crime-scene sample, then the average probability that the database search attributes the crime-scene sample to a wrong person is ( N  −  d ) p _A .     

Comparison of the elemental composition of office document paper: evidence in a homicide case

Fraudulent substitution of a page within a multiple page document such as a will or business contract, the counterfeit manufacture of paper banknotes, and linking ransom or extortion notes have all been the focus of criminal investigations at one time or another. In a recent homicide investigation, document examiners were requested to compare a threatening letter received by a business partner of the deceased with paper samples seized under warrant from a suspect's house. Through a quantitative elemental analysis of the concentrations of nine elements (Na, Mg, Al, Mn, Sr, Y, Ba, La, and Ce) within the questioned and specimen documents, determined by inductively coupled plasma-mass spectrometry (ICP-MS), it was concluded that (i) the paper of the threatening letter originated from a different source to that of the paper seized from the suspect's house and (ii) all six pages of paper seized from the suspect's house originated from the same source. This discrimination of paper is presented as both a statistical t-test analysis (99.9% confidence limit) as well as construction of an elemental fingerprint for individual replicates within the questioned and specimen sample populations. This is the first reported use of the comparison of the elemental composition of document paper, determined by ICP-MS, to assist in a criminal investigation.     

Multicolor Real-Time PCR Genotyping of ABO System Using Displacing Probes

Abstract:  Rapid and informative ABO genotyping has become increasingly popular in forensic use. We developed a multiplex real-time polymerase chain reaction (PCR) approach to genotype ABO major groups and subgroups. Seven differently fluorophor-labeled displacing probes for O¹(261delG), A(261G), A(796C/803C), B(796A/803C), O² (802G>A), A² (1059delC), and A² (1009A>G) were combined in one or two PCRs to determine either ABO major groups or subgroups. The method correctly detected 13 reference DNA samples. A blind test of 237 samples resulted in complete agreement with their phenotypes, and 110 of these 237 samples as well as with PCR-SSP method. The whole analysis could be finished in less than 100 min at substantially low material cost and the template DNA ranging from 0.16 to 500 ng per reaction could be quantitatively detected. Despite the limited informativeness of ABO genotyping, the developed methods could find application in rapid and inexpensive screening of forensic settings.     

玻璃中痕量金属元素检测方法研究

目的建立玻璃中金属元素的快速检测方法。方法采用高温消解法对样品进行预处理,用电感耦合等离子体发射光谱仪同时对多种金属元素进行检测,同时对方法的精密度和准确度进行了测定。结果采用氢氟酸对样品进行预处理,各元素同时测定的发射光谱图相互无干扰。在所设定的条件下,各种元素的回收率均〉75％,相对标准偏差均〈10％。结论玻璃中金属元素可以通过高温消解进行预处理,应用电感耦合等离子体发射光谱仪同时进行检测。     

Elemental analysis of white cotton fiber evidence using solution ICP-MS and laser ablation ICP-MS (LA-ICP-MS)

The purpose of this research is to investigate a method for the forensic elemental analysis of cotton fibers for the purpose of increasing the discrimination between otherwise similar cotton evidence using microwave digestion inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). A quadrupole ICP-MS and UV laser ablation (266 nm) instruments were used for the analysis. A cotton standard reference material (IAEA V-9) was used to validate the developed methods producing good accuracy with typically <10% bias and good precision (typically <5% RSD) for the element list: ²⁵Mg, ²⁷Al, ⁵⁵Mn, ⁵⁷Fe, ⁸⁸Sr and ¹³⁷Ba. It was found that the LA-ICP-MS method resulted in improved precision over the solution ICP-MS method. Twenty-four raw cotton samples and five white cotton T-shirts were analyzed with the developed methods. It was also found that all the raw cotton samples from different sources were distinguishable from each other, as were all the cotton T-shirts resulting in zero type I errors and zero type II errors for the pairwise comparisons. The laser ablation method was slightly faster than the solution-based analysis, requiring 3 h for the laser analysis of 10 samples vs. 3.5 h for the solution analysis, including sample preparation time. One additional advantage of the LA-ICP-MS method was the extremely low sample consumption (1.75 μg were consumed vs. 250 mg for the solution-based method) and the fact that the LA samples are amenable for reanalysis.     

Elemental analysis of 3,4-methylenedioxymethamphetamine (MDMA): A tool to determine the synthesis method and trace links

The elemental composition of 3,4-methylenedioxymethamphetamine (MDMA) powders and tablets was determined. The objective was the identification of the synthesis method and application of the elemental profile in comparative analysis. The developed analytical method comprised the digestion of a sample followed by quantitative analysis with inductive coupled plasma mass spectrometry (ICP-MS) and inductive coupled plasma atomic emission spectroscopy (ICP-AES). The sample collection consisted of a unique set of MDMA powders (57) from illicit production sites and MDMA tablets (97) taken from large seizures (over 500 tablets) in the Netherlands. The production method of MDMA could be determined for 89 of the 97 tablets. In 84 cases reductive amination using Pt as the catalyst was used, in four cases reductive amination using NaBH(4) or a similar reducing agent was employed and one mixed sample (Pt and B) was found. None of the MDMA tablets were assigned to the aluminium amalgam method. Using the elemental profile, 13 links were identified within the 97 MDMA tablets using cluster analysis based on Pearson correlations. Of these links 10 were corroborated by additional analyses.     

Compensation for Commercial Agents

This note examines the decision of the House of Lords in Lonsdale (t/a Lonsdale Agencies) v Howard & Hallam Limited ¹ where the House of Lords were asked to rule on the correct method to be applied when calculating the compensation of commercial agents ² under Regulation 17 of The Commercial Agents (Council Directive) Regulations 1993 ³ (the Regulations). This ruling settles this aspect of the law in England and Wales after almost fifteen years of legal and commercial uncertainty on the matter.     

Secondary Iatrogenic Harm: Claims for Psychiatric Damage Following a Death Caused by Medical Error

The purpose of this paper is to investigate the feasibility of claims for psychiatric damage following the death of a family member, where that death has been caused by medical error. ¹ The relative's position is a subject of heightened interest since the exposure of the plight of the parents involved in the UK organ scandal, ² and in the case of an iatrogenic death it is, of course, the family who are essentially the focus of the law's attempts to provide redress. Whilst the cases of deceased patients' relatives seeking damages for mental harm are inherently problematic in light of the restrictive secondary victim criteria applicable to psychiatric damage claims, a close look at the rules which permeate this area of compensation reveals that denying compensation to the relative suffering psychiatric harm is difficult to sustain. ³     

Identification of cremains using X-ray diffraction spectroscopy and a comparison to trace element analysis

The ability to distinguish human cremains from filler materials can be important in a variety of situations, the most notorious recent example being the Tri-State Crematorium incident. However, the majority of the papers in the recent literature present methods that rely on trace or minor element analysis, usually followed by a statistical or variable cluster analysis, to determine attribution. This approach is inherently risky, as there is significant natural variation in the trace and minor element body burdens within the human population and no real baseline for comparison. Bones and teeth are a form of calcium phosphate that is part of the mineral group apatite, often referred to as bioapatite. X-ray diffraction (XRD) spectroscopy is a technique that is used to identify minerals by their crystalline structures rather than their elemental composition. The members of the mineral group apatite have a highly flexible hexagonal (6/m) structure that is able to incorporate small amounts of a wide variety of elements. However, its structure, and therefore its X-ray diffraction pattern, is distinct from the crystalline structures of all of the commonly reported filler materials, most of which are composed of some combination of Portland cement, limestone aggregate and quartz sand. XRD has several advantages over other analytical techniques for the identification of cremains. It is non-destructive, requires relatively small amounts of material, is unaffected by the elemental variations found in bioapatite, and can be used to semi-quantify the components of a mixture, thus determining the relative level of contamination of a sample. This paper presents the results of X-ray diffraction spectroscopy analysis of human cremains and a variety of common filler materials.     

微波消解ICP-MS法测定人发中的汞

目的建立人发中汞的电感耦合等离子体质谱分析方法。方法采用微波消解法处理样品,以铟（115In）作内标,用电感耦合等离子体质谱分析人发中的汞含量。结果方法检出限为0.0032μg/g,准确度通过测定人发标准物质GBW07601、GBW09101b进行验证,检测结果与标准参考值相符。结论该方法快捷、高效,灵敏度、准确度高,适用于人发中汞含量的检测。     

The Stable Isotope Ratios of Marijuana. II. Strontium Isotopes Relate to Geographic Origin

Abstract:  Effectively addressing marijuana trade is aided by understanding marijuana geographic sources. We analyzed the ⁸⁷Sr/⁸⁶Sr of marijuana samples grown in 79 counties across the United States to determine if a primary geologic signal is retained in marijuana, which could therefore be useful for geographic sourcing. The marijuana results were compared with modeled bedrock ⁸⁷Sr/⁸⁶Sr values based on ⁸⁷Rb decay rates and a generalized geologic map of the U.S.A. A significant correlation was observed between marijuana ⁸⁷Sr/⁸⁶Sr and modeled bedrock ⁸⁷Sr/⁸⁶Sr. Although values clustered near the 1:1 relationship, there was a predominance of positive anomalies, perhaps attributable to carbonate bedrock. A small number of negative anomalies were also observed, which were generally associated with granitic bedrocks. These results suggest that strontium isotopes in marijuana record the geographic origins of marijuana, and that refinement of the base strontium map (or strontium isoscape) and improved understanding of other strontium sources would be productive.     

A Multi-Drug Intoxication Fatality Involving Xyrem® (GHB)

Abstract:  Gamma-hydroxybutyrate (GHB) is best known as a recreational depressant drug, whose use has also been implicated in drug facilitated sexual assault cases. It is also available as a therapeutic agent (Xyrem^®) used for the treatment of daytime sleepiness or cataplexy associated with narcolepsy. This is a report of a case of a 53-year-old woman undergoing treatment with Xyrem^® for narcolepsy. The decedent was also prescribed tramadol, gabapentin, cetirizine, modafinil, carisoprodol, and Xyrem^®. Toxicological analysis of the blood revealed GHB 165.6 mg/L, and 90.7 mg/L in the urine. Blood GHB concentrations in the range 156–260 mg/L have been reported to induce moderately sound sleep. The combined use of central nervous system depressant drugs, together with her problematic sleep apnea, and snoring (both contraindications for GHB use) were determined to have caused this subject's death. The manner of death was determined to be accidental.     

The Use of Hemastix® and the Subsequent Lack of DNA Recovery Using the Promega DNA IQTM System

Abstract:  Following implementation of our automated process incorporating the Promega DNA IQ^TM system as a DNA extraction method, a large number of blood-containing exhibits failed to produce DNA. These exhibits had been tested with the Hemastix^® reagent strip, commonly used by police investigators and forensic laboratories as a screening test for blood. Some exhibits were even tainted green following transfer of the presumptive test reagents onto the samples. A series of experiments were carried out to examine the effect of the Hemastix^® chemistries on the DNA IQ^TM system. Our results indicate that one or more chemicals imbedded in the Hemastix^® reagent strip severely reduce the ability to recover DNA from any suspected stain using the DNA IQ^TM magnetic bead technology. The 3,3',5,5'-tetramethylbenzidine (TMB) used as the reporting dye appears to interact with the magnetic beads to prevent DNA recovery. Hydrogen peroxide does not seem to be involved. The Hemastix^® chemistries do not interfere in any way with DNA extraction performed using phenol-chloroform. The incompatibility of the Hemastix^® chemistries on the DNA IQ^TM system forced us to adopt an indirect approach using filter paper to carry out the presumptive test.     

Using morphometric and analytical techniques to characterize elephant ivory

There is a need to characterize Asian elephant ivory and compare with African ivory for controlling illegal trade and implementation of national and international laws. In this paper, we characterize ivory of Asian and African elephants using Schreger angle measurements, elemental analysis {X-ray fluorescence (XRF), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and inductively coupled plasma-mass spectroscopy (ICP-MS)} and isotopic analysis. We recorded Schreger angle characteristics of elephant ivory at three different zones in ivory samples of African (n=12) and Asian (n=28) elephants. The Schreger angle ranged from 32 degrees to 145 degrees and 30 degrees to 153 degrees in Asian and African ivory, respectively. Elemental analysis (for Asian and African ivory) by XRF, ICP-AES and ICP-MS provided preliminary data. We attempted to ascertain source of origin of Asian elephant ivory similarly as in African ivory based on isotopes of carbon, nitrogen and strontium. We determined isotopic ratios of carbon (n=31) and nitrogen (n=31) corresponding to diet and rainfall, respectively. Reference ivory samples from five areas within India were analyzed using collagen and powder sample and the latter was found more suitable for forensic analysis. During our preliminary analysis, the range of delta13C values (-13.6+/-0.15 per thousand and -25.6+/-0.15 per thousand) and delta15N values (10.2+/-0.15 per thousand and 3.5+/-0.15 per thousand) were noted.     

WILLIAM H. REHNQUIST AWARD ADDRESS

The William H. Rehnquist Award is one of the most celebrated judicial honors in the country. ¹ It is given each year to a state court judge who demonstrates the "highest level of judicial excellence, integrity, fairness, and professional ethics." ² The 2004 recipient, Judge Leonard Edwards, is the Supervising Judge of the Santa Clara County, California juvenile dependency court. ³ He is the first juvenile court judge to receive this prestigious award. During the 24 years he has held his position, Judge Edwards has worked extremely hard to improve how the juvenile court system serves troubled families. He has founded two organizations to achieve this end, the Juvenile Court Judges of California and the Santa Clara County Domestic Violence Council. ⁴ Judge Edwards serves as a lead judge in San Jose's Model Court, which is one of twenty-five jurisdictions in the country which utilizes new ideas and techniques to improve adoption rates for children in foster care. ⁵ Moreover, he has worked as president of the National Council of Juvenile and Family Court Judges. ⁶ Below is the speech he gave after accepting the award from U.S. Supreme Court Justice Anthony M. Kennedy. The speech notes the importance of the award to everyone working in America's juvenile courts.     

Concordance Between the AmpFℓSTR® MiniFiler™ and AmpFℓSTR® Identifiler® PCR Amplification Kits in the Kuwaiti Population

Abstract:  The AmpFℓSTR^® MiniFiler™ polymerase chain reaction amplification kit, developed and supplied by Applied Biosystems, complements the AmpFℓSTR^® Identifiler^® polymerase chain reaction amplification kit (Applied Biosystems, Warrington, U.K.) by improving the success rate when profiling DNA that is degraded or contains inhibitors. Before applying the MiniFiler™ kit to casework, the profiles from 200 unrelated Kuwaitis were compared to Identifiler^® profiles. Concordance was observed for 99.875% (1598 of 1600) of the compared STR loci. The two discordant profiles displayed allelic dropout: one at the D13S317 locus due to nonamplification of allele 10 in the MiniFiler™ profile, and one at the D18S51 locus due to nonamplification of allele 18 in the Identifiler^® profile.     

The Effect of Buscopan® on the Development of the Blow Fly Chrysomya megacephala (F.) (Diptera: Calliphoridae)

Abstract:  This work investigated the effects of butylscopolamine bromide, a drug present in the pharmaceutical formulation Buscopan^®, on the development of Chrysomya megacephala , a blow fly species of considerable forensic and medical importance in Brazil. Larvae exposed to the drug showed a decreased rate of development, with higher drug concentrations further retarding the development. Besides, larvae reared on the presence of the drug showed smaller body weight and body length when compared with larvae reared on the absence of Buscopan^®. The drug also affected the mortality of the species.     

微波消解ICP-MS法检测生物检材中汞元素

目的 建立生物检材中汞的电感耦合等离子体质谱分析方法.方法 采用微波消解法处理样品,以铟(115In)作内标,用电感耦合等离子体质谱仪对血液、尿液和头发中的汞含量进行分析.选择金与汞形成金汞齐,对金消除汞记忆效应的能力进行考察.结果 方法检出限为0.01μg/L,准确度为97.0%～107.1%.检测中添加金质量浓度在...