Field-portable detection of fentanyl and its analogs: A review

The need to detect fentanyl and its analogs in the field is an important capability to help prevent unintentional exposure or overdose on these substances, which may result in death. Many portable methods historically used in the field by first responders and other field users to detect and identify other chemical substances, such as hazardous materials, have been applied to the detection and identification of these synthetic opioids. This paper describes field portable spectroscopic methods used for the detection and identification of fentanyl and its analogs. The methods described are automated colorimetric tests including lateral flow assays; vibrational spectroscopy (mid-infrared and Raman); gas chromatography–mass spectrometry; ion mobility spectrometry, and high-pressure mass spectrometry. In each case the background and key details of these technologies are outlined, followed by a discussion of the application of the technology in the field. Attention is paid to the analysis of complex mixtures and limits of detection, including the required spectral databases and algorithms used to interrogate these types of samples. There is also an emphasis on providing actionable information to the (likely) non-scientist operators of these instruments in the field.     

A longitudinal analysis of technical communication in research and development

A unique longitudinal study of the technical communication patterns of 184 engineers in a high technology research and development laboratory centers in the activities of technology gatekeepers. This two-step flow of technical information follows the literature as well as results from prior studies. Gatekeepers span the organizational boundary in the transfer of technology from outside the laboratory, while facilitating the distribution of technical information to colleagues within the organization. Sociometric data are analyzed over a five-year period with respect to changing organizational structures, new technical assignments and alterations in group composition. Despite these dynamic changes, the data reveal consistent results in gatekeeper identification and technical information flows.     

The detection of psilocin in human urine

Pharmacokinetic studies of psilocybin in humans have shown the rapid dephosphorylation of psilocybin to psilocin with further conversion to 4-hydroxy-tryptophole (4HT) and 4-hydroxyindole-3-acetic acid (4HIAA) in plasma. Our study shows that psilocin also undergoes conjugation and can be found in the urine as the psilocin-glucuronide conjugate. Recoveries after enzymatic hydrolysis of the urine with beta-glucuronidase (Helix Pomatia or E. Coli) when compared to non-hydrolyzed urine confirmed the presence of the glucuronide. Detection of psilocin from hydrolyzed and extracted samples was optimized for GC/MS by derivatization with MSTFA. The method developed allows for the detection of psilocin in urine with a limit of quantitation of 10 ng/mL, based on 5 mL of spiked urine. Using this method, our laboratory has confirmed the presence of psilocin in 6 out of 8 urine samples, with concentrations ranging from 10 ng/mL to greater than 200 ng/mL. Before implementation of the hydrolysis and derivatization steps, our limit of detection was 200 ng/mL, based on spiked urine standards. No case samples were positive without hydrolysis and derivatization.     

SPME-GC-MS法快速检测尿液中的甲基苯丙胺

目的建立SPME-GC-MS快速检测吸毒人员尿液中的甲基苯丙胺的方法。方法以SPME法提取尿液中的甲基苯丙胺,以1-萘胺作内标,用GC-MS法检测。结果在2～2000ng/mL的范围内呈线性关系(r=0.9985,n=7),甲基苯丙胺的检测限为0.5ng/mL(信噪比3),在低、中、高(200、500、1000ng/mL)浓度的平均相对回收率为102.6%、98.5%、93.2%,日内及日间RSD分别小于8.1%、7.2%。结论用此方法检测尿液中的甲基苯丙胺,灵敏度高,简单快速,易操作,适用于吸毒人员的快速定性定量检测。     

Methodology and interpretation of morphiate detection in urine samples

In TLC screenings of 335 urine samples taken because of suspicion of heroin consumption, positive evidence of morphine was found in about 50% of the cases, which was confirmed without exception by gas chromatography-mass spectrometry. In 66% of the positive cases, morphine and codeine were found; in about 31% only morphine was found, and the median value of 0.4 mg/l free morphine and 1.0 mg/l conjugated morphine was considerably lower than in the whole collection of samples. Comparison of the codeine/morphine quotients (Q), especially the free bases, proves that the groups of heroin/morphine or codeine consumers can be distinctly differentiated. The critical conditions of the conjugated bases worked out by Dutt et al. (1983) proved to be right. Using the equation Qf less than 0.5 square root c, a boundary condition for the free flare bases can also be developed, which is dependent on the sum of the codeine and morphine concentrations and which proves heroin/morphine consumption with 98% certainty.     

A novel method for GHB detection in urine and its application in drug-facilitated sexual assaults

A confirmation procedure for the identification and quantification of gamma-hydroxybutyric acid (GHB) in urine is presented. This method is unique in that it does not involve the conversion of GHB to the gamma-butyrolactone (GBL). The urine samples were extracted using ethyl acetate, evaporated and derivatized with N, O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS), and analyzed by gas chromatography-mass spectrometry. Quantification was performed using selective ion monitoring (SIM), using GHB-d(6) as the internal standard. This method is simple and provides excellent linearity and sensitivity for GHB in urine.     

The detection of group-specific component from urine samples

The detection of group-specific component (Gc) from serum and bloodstains has been widely used in the forensic laboratory. A recent increase in substituted or adulterated urine samples in various drug screening programs has necessitated methods to determine the donor. This paper discusses the detection of Gc from urine samples. The samples were concentrated and applied to ultrathin polyacrylamide gel and focused for 150 min. This method separates the samples into the three common phenotypes found in all human populations. A nitrocellulose membrane blotting technique was used to detect the Gc bands. Serum and urine samples were collected from each individual and were typed for Gc. Urine samples tested after 6 months of storage (4 degrees C) were still readable. This method provides the forensic laboratory with an additional test from a body fluid which, until recently, provided little information.     

芬太尼中毒死亡大白兔体内分布研究

目的建立芬太尼中毒致死的动物模型,探讨芬太尼在致死大白兔体内的分布规律。方法用6只雄性大白兔按5.4mg/kg(2LD50)经耳缘静脉推注芬太尼注射液,大白兔死后迅速解剖并提取心、肝、脾、肺、肾、脑、肌肉、睾丸、胃、心血、周围血、胆汁和尿液,用正己烷∶乙醇(20∶1)萃取,利用UPLC-MSn法检测各组织和体液中芬太尼含量,使用SPSS15.0进行方差分析,均数两两比较的SNK法进行统计分析。检验水准为α=0.05。结果实验大白兔给药后1min出现颈项强直、四肢抽搐等中毒症状,平均4.7min因呼吸抑制而死亡。死后肺内芬太尼含量最高,其次是肾和心,而尿液中含量较低。结论本实验的结果与相关案例报道基本吻合,提示肺、肾和心脏是芬太尼中毒案件鉴定的理想检材,芬太尼在致死大白兔体内的分布规律可为相关案件的鉴定提供一定的依据。     

Comparison of nonradioactive microtiter plate enzyme immunoassays for the sensitive detection of fentanyl

Fentanyl is a very strong opioid with analgesic properties that are approximately 80 times stronger than those of morphine and therefore is used in major surgery and treatment of pain in tumor patients. Cases of fentanyl abuse by intravenous injection, inhalation, oral or nasal application have been reported especially in the USA. Therapeutic levels of fentanyl are as low as 1 ng/ml of serum and therefore a screening test must have a detection limit below that concentration. Recently three non-radioactive enzyme immunoassays (EIAs) have become commercially available from COZART, STC and DIAGNOSTIX, all of them supplied by MAHSAN Diagnostika for evaluation with serum samples from forensic and clinical cases. A calibration curve is obtained with samples that contain 0, 0.1, 0.5, 1 and 5 ng fentanyl per ml of negative serum. The calibration curve of COZART is especially in the low range, steeper than those of STC and DIAGNOSTIX. The cut-off for all these EIAs, however, can be set at 0.5 ng/ml. After the administration of therapeutic doses, fentanyl concentrations were between 3 and more than 5 ng/ml as determined with the EIAs. The presence of the typical drugs of abuse, e.g. heroin, methadone, cocaine, cannabinoids and amphetamines including the derivatives of methylenedioxyamphetamine, don't generate false-positive results. No cross-reactivity was also observed at toxic levels of benzodiazepines and paracetamol and therapeutic levels of barbiturates, phenothiazines, antidepressants and analgesics. The EIAs tested so far appear to be suitable for the detection of fentanyl at therapeutic levels. False-positive results or cross-reactivity towards other compounds have not been observed.     

The detection of hydromorphone in urine specimens with high morphine concentrations

A previous study suggested that small amounts of morphine are metabolically converted to hydromorphone. In the present study, morphine positive urine specimens obtained from a postmortem laboratory and a random urinalysis program were tested for morphine, codeine, hydromorphone, hydrocodone, oxymorphone, and oxycodone to assess the possibility that small amounts of hydromorphone are produced from the metabolism of morphine. The opioids were analyzed by gas chromatography-mass spectrometry as their respective trimethylsilyl derivatives following solid phase extraction. The limit of detection for hydromorphone was 5 ng/mL. A total of 73 morphine positive urine specimens were analyzed, with morphine concentrations ranging from 131 to 297,000 ng/mL. Hydromorphone was present at a concentration > or =5 ng/mL in 36 of these specimens at concentrations ranging from 0.02% to 12% of the morphine concentration. Hydrocodone was not detected in these specimens at the assay detection limit of 25 ng/mL. These results support earlier work suggesting that the detection of hydromorphone in urine specimens does not necessarily mean that exogenous hydromorphone or hydrocodone was used.     

Passive exposure in detection of low blood and urine cannabinoid concentrations

Whenever small amounts of drugs are present in blood or urine samples, especially of substances that are preferentially smoked such as cannabinoids, the discrimination between active and passive inhalation may cause severe problems. The statement of a passive exposure by marijuana smoke has been scrutinized reviewing the literature. The pharmacokinetics of smoked marijuana as well as experimental data on cannabinoid concentrations in plasma and urine samples following passive exposure are summarized. As a conclusion it seems urgent to enlarge the existing data base.     

Fatal intravenous fentanyl abuse: four cases involving extraction of fentanyl from transdermal patches

The transdermal fentanyl system delivers a specific dose at a constant rate. Even after the prescribed application time has elapsed, enough fentanyl remains within a patch to provide a potentially lethal dose. Death due to the intravenous injection of fentanyl extracted from transdermal patches has not been previously reported. We present 4 cases in which the source of fentanyl was transdermal patches and was injected. In all of these cases, the victim was a white male who died at home. Case 1 was a 35-year-old with no known history of drug use, who was found by his wife on the floor of his workshop. Police recovered a fentanyl patch, needle, and syringe at the scene. Case 2 was a 38-year-old with a known history of drug use whose family claimed that he was in a treatment program that used fentanyl patches for unknown reasons. His brother found him dead in bed, and law enforcement officers found a hypodermic needle beside the body; a ligature around his left hand, and apparent needle marks between his first and second digits were also noted. Case 3 was a 42-year-old with a recent attempted suicide via overdose who was found dead at his home. An empty box of fentanyl patches, Valium, Ritalin, and 2 syringes were found at the scene. Case 4 was a 39-year-old found by his mother, who admitted to removing a needle with attached syringe from the decedent's arm. Medications at the scene included hydrocodone, alprazolam, zolpidem, and fentanyl patches. All reported deaths were attributed to fentanyl intoxication, with blood concentrations ranging from 5 to 27 microg/L.     

A brief study of time

In this paper we describe the first large-scale, long-term study of how hosts connected to the Internet manage their clocks. This is important for forensic investigations when there is a need for correlation of events collected from disparate sources, as well as for the correlation of computer events to “real” time. We have sampled over 8000 web servers on the Internet on a regular basis for a period of over six months. We have found that only about 74% of the hosts we observed were within 10 s of our reference time (UTC). The other hosts exhibited a large variety of different clock behaviors, some of which are explainable by existing clock models, some not, warranting further research in the area of forensic time and clock analysis.     

Windows of detection of zolpidem in urine and hair: application to two drug facilitated sexual assaults

A LC-MS/MS method for the detection of zolpidem in hair was developed to detect this drug after a single dose in possible drug facilitated sexual assaults. To determine the window of detection of zolpidem in both urine and hair, three volunteers received a 10 mg dose. Urine specimens were collected each 12 h for 144 h. Hair was sampled 3-5 weeks after exposure. Hair and urine extracts were separated on a Xterra MS C18 column using a gradient of acetonitrile and formate buffer. For each compound, detection was related to two daughter ions. Zolpidem was detected for up to 60 h in urine with peak concentrations obtained at 12 h. A single exposure to zolpidem was detected in hair at concentrations ranging from 1.8 to 9.8 pg/mg. Hair analysis was applied to two possible criminal cases. In the first case, zolpidem tested positive in the corresponding hair segment at 4.4 pg/mg. In the other case, zolpidem was detected in all the segments analyzed, demonstrating likely previous drug use in addition to recent exposure associated with a positive blood result.     

顶空固相微萃取气相色谱法快速检测尿液中氯胺酮

目的建立快速检测吸毒人员尿液中氯胺酮的顶空固相微萃取(HS/SPME)-GC/NPD的方法。方法样品瓶中加入尿液、氢氧化钠溶液、氯化钠,在95℃下加热搅拌,用聚二甲基硅氧烷SPME萃取头(100μm)顶空萃取20min,气相色谱氮磷检测器检测,外标法定量。结果尿液中氯胺酮浓度在0.2~20.0μg/ml范围内呈现线性关系(r2=0.9965),尿液添加1.0μg氯胺酮,平均回收率102.6%,RSD=3.39%(n=7),检测限1.13ng/ml(S/N=3)。结论建立的方法简单、快速、灵敏、准确,十分适合尿液等生物检材中氯胺酮的快速定性定量分析。     

尿中吗啡的氮磷检测——气相色谱分析法

目的建立尿中吗啡的简便快速、灵敏可靠的GC/NPD分析方法。方法样品尿加内标烯丙吗啡,酶或酸催化水解,氯仿-异丙醇(9:1)液液提取或GDX403树脂固相提取,BSA衍生化,HP-5柱和氮磷检测器进行分析。结果 提取率62％～85％,检出限1.2～3.1ng/ml,线性范围20～2000ng/ml,回收率(97％～99％)±(6％~9％)(Mean±cv,N=5)。结论 方法适合于实际案件中尿样的检验。     

ELISA detection of clonazepam and 7-aminoclonazepam in whole blood and urine

The ability of five commercially available enzyme-linked immunosorbent assay (ELISA) benzodiazepines to detect clonazepam and 7-aminoclonazepam in blood and urine was investigated. To determine the cross-reactivity of various ELISA assays, drug free blood and urine were fortified with clonazepam and 7-aminoflunitrazepam at concentrations of 1, 2.5, 5, 10, and 25microg/dl. The cross-reactivity, with respect to oxazepam, for clonazepam was 16, 37, 80, 93, and 109% with Immunalysis, Diagnostix, Neogen, OraSure, and Cozart, respectively; for 7-aminoclonazepam, none of the five ELISA assays showed any cross-reactivity above 10%.     

A brief overview of quantitative criminology in Australasia: 1981–1995

This paper reviews quantitative criminological research, especially of a sophisticated mathematical nature, published by researchers in Australia and New Zealand since 1981. A statistical analysis of quantitative articles published between 1981 and 1995 in the leading academic journal.The Australian and New Zealand Journal of Criminology, showed that using the five topical categories developed by Farrington (this issue), there has been little change in the types of research carried out, with studies of court processes and correctional issues accounting for two-thirds of papers. The numbers of “simple” and ”sophisticated” quantitative articles as proportions of the total published also did not vary over the 15 years. Areas of strength in quantitative research include drugs, alcohol, and crime; indigenous peoples and the criminal justice system; regulatory law enforcement; the modeling of recidivism; and sentencing. Most sophisticated quantitative research is carried out by noncriminologists, and it appears unlikely that the amount of mathematically sophisticated research will increase significantly in the next few years. Experimental studies and longitudinal designs will probably slowly grow in popularity, and crime prevention will emerge as an area of quantitative strength.     

Swedish quantitative criminology in the 1990s: A brief overview

Quantitative criminology research published in Sweden in the 1990s is reviewed and put in the context of major Swedish traditions in quantitative criminological research. Sweden has a strong tradition in sophisticated longitudinal and ecological research which continues into the 1990s. Other traditionally prominent areas of Swedish quantitative research include studies of crime trends, violence, and youth criminality. Traditionally Swedish quantitative criminology has been dominated by studies using official statistics and criminal records as data. In the 1990s there has been a significant upswing in survey studies, motivated partly by an increased interest in questions of etiology and crime prevention. More fundamental research on the causes of crime, including new longitudinal studies, and more evaluations of crime prevention initiatives are needed.