血液1-(3-三氟甲基苯基)哌嗪和1-(3-氯苯基)哌嗪检验

目的建立血液中1-(3-三氟甲基苯基)哌嗪(TFMPP)、1-(3-氯苯基)哌嗪(m CPP)的检测方法,并用于实际案件检验。方法 Zn SO4沉淀蛋白后,在p H11条件下,用氯仿/异丙醇(4/1,v/v)提取,采用GC/MS与GC/NPD分析。结果 TFMPP、m CPP回收率均在90%以上,在0.25~20μg/m L浓度范围内线性关系良好,r2为0.999 9,最低检测限为0.135μg/m L。结论本方法回收率高,操作简便,可用于血液中TFMPP、m CPP的提取检测。     

液相色谱-三重四级杆/线性离子阱串联质谱法测定血液中1-(4-甲氧基苯基)哌嗪

目的建立血液中1-(4-甲氧基苯基)哌嗪的液相色谱-三重四级杆/线性离子阱串联质谱(LC-QTrap-MS/MS)的快速检测方法。方法血液经乙腈沉淀蛋白后,振荡、离心、经微孔滤膜过滤后供仪器分析;选用Phenomenex Kinetx®5.0μm Biphenyl 100Å(100mm×2.1mm)分离,柱温40℃;以0.1%甲酸水溶液-乙腈为流动相,流速0.5mL/min,梯度洗脱5.5min;以多反应监测(MRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)-谱库检索的模式进行分析,外标-标准曲线法进行定量分析。结果血液中1-(4-甲氧基苯基)哌嗪的浓度在2~200ng/mL范围内呈现良好的线性关系,相关系数达到0.9984,回收率在87%以上,日内精密度在5%以下,日间精密度在10%以下,方法的检出限是0.8ng/mL,定量限是2ng/mL。结论该方法采用LC-QTrap-MS/MS和MRM-IDA-EPI模式,既保持与MRM相同的定量灵敏度,也能提供更为丰富的二级质谱碎片,使定性结果更加准确。方法简单快捷,专属性好,回收率高,重现性好,能够用于血液中1-(4-甲氧基苯基)哌嗪同时定性和定量分析。     

超高效液相色谱串联质谱法同时快速检验血液中3种哌嗪类新型毒品

目的建立血液中3种哌嗪类新型毒品超高效液相色谱-三重四级杆质谱(UPLC-TQ/MS)快速检验方法。方法采用固相支撑液液萃取前处理方法,全血样品过柱后,用乙酸乙酯进行洗脱,氮吹浓缩后用初始流动相定容,Waters T3色谱柱分离,0.1%甲酸水和乙腈进行梯度洗脱。采用电喷雾电离,正离子(ESI+)模式扫描,多反应监测(MRM)模式检测。结果三种药物在1～500 ng/mL范围内呈良好线性关系(R~2≥0.999),回收率为92.3%～105.3%,相对标准偏差为0.7%～3.7%,方法检出限(S/N=3)为0.04～0.13 ng/mL,定量限(S/N=10)在0.13-0.43 ng/mL范围内。结论该方法能够满足实际办案快速、准确的需求。     

GC／MS检验1-苯基-1-丙酮和1-苯基-2-丙酮

目的阐明1-苯基-1-丙酮和1-苯基-2-丙酮在色谱行为、用途和受管制程度等方面的差异。方法使用GC／MS对1-苯基一1-丙酮和1-苯基-2-丙酮进行定性分析。结果1-苯基-1-丙酮和1-苯基-2-丙酮的保留时间相差约1min，特征离子显著不同。结论1-苯基-1-丙酮和1-苯基-2-丙酮虽然为同分异构体，且多数时中文名称都简称为苯丙酮，也都是制备毒品的原料，但其实二者在色谱行为、用途、管制程度上却有着巨大的差别。     

新型毒品1-（3-三氟甲基苯基）哌嗪的检验

目的建立新型毒品1-（3-三氟甲基苯基）哌嗪的检验方法。方法通过选择和优化建立了1-（3-三氟甲基苯基）哌嗪类毒品的GC／MS、GC／TSD定性定量分析条件。结果以建立的分析方法,知查获的片剂中含有1-（3-三氟甲基苯基）哌嗪,其含量为51．13％,GC／TSD最低检出线是10ng／mL。结论本文所建方法可以用于1-（3-三氟甲基苯基）哌嗪涉毒检材的检验鉴定。     

自主合成标准物质鉴定缴获物中的新精神活性物质ADB-FUBINACA

目的新精神活性物质在世界范围内蔓延迅速,但相关标准物质的短缺制约着其分析方法的研究和案件检验。本文以我国首次出现的N-(1-氨甲酰基-2,2-二甲基丙基)-1-(4-氟苄基)吲唑-3-甲酰胺(ADB-FUBINACA)制毒案件为例,介绍在无法及时获得商业化标准物质的情况下,不得不通过自主合成制备标准物质解决案件检验难题,建立该新精神活性物质检验的方法。方法建立气相色谱-质谱检验方法,分析条件:色谱柱为Aglient DB-5MS石英毛细管柱(30.00m×0.25mm×0.25μm);初始柱温60℃,按15℃/min升至300℃,保持15min;载气为氦,流速1.0mL/min,分流进样,进样量1.0μL,分流比20∶1;进样口温度280℃;电子轰击(EI)离子源,电子能量70eV,离子源温度230℃,四级杆温度150℃,传输线温度280℃,质量扫描范围m/z 40~500amu,全扫描模式(SCAN)采集总离子流图,溶剂延迟3.0min。案件缴获的送检未知样品经甲醇提取,超声、离心后,取上清液以GC-MS分析;将所得主要质谱特征碎片峰(m/z)通过NIST质谱库、SWGDRUG质谱数据库以及相关文献进行检索,初步确定待测目标物。采用有机合成技术制备ADB-FUBINACA标准物质,合成路线为:吲唑-3-甲酸甲酯与4-氟苄溴发生取代反应,生成1-(4-氟苄基)-1H-吲唑-3-甲酸甲酯;取代产物在碱性条件下经水解反应得到有机酸1-(4-氟苄基)-1H-吲唑-3-甲酸;在催化剂作用下,有机酸与L-叔亮酰胺发生酰化反应,制得化合物ADB-FUBINACA。经气相色谱-质谱(GC-MS)、液相色谱-离子阱-飞行时间质谱(LCMS-IT-TOF)、核磁共振(NMR)等分析,合成化合物的结构得以确证;同时采用超高效液相色谱-二极管阵列检测器(HPLC-PDA)进行分析,对其归一化纯度进行测定。将案件未知样品和合成标准物质分别用甲醇提取,超声、离心后,再行上清液GC-MS分析。结果经GC-MS分析,案件未知样品(RT=19.818min)的质谱特征碎片峰(m/z)信息为109.0(基峰)、253.1、338.1、309.1和145.0,经与合成标准物质的保留时间及质谱图检测比对,证实为N-(1-氨甲酰基-2,2-二甲基丙基)-1-(4-氟苄基)吲唑-3-甲酰胺;通过查阅相关资料,对上述质谱特征碎片峰的产生机制进行了推断,并对1H-NMR、13C-NMR和DEPT-135等一维核磁谱图的信号进行了归属分析。结论本文报道的新精神活性物质ADB-FUBINACA其GC-MS分析方法,可用于实际案件检验鉴定;合成化合物的结构表征方法也可用于固体ADB-FUBINACA的定性分析。基于有机合成技术的新精神活性物质制备与案件检验方法,可缓解有关标准物质短缺制约该类案件检验鉴定的现状。     

缴获物中2-(2-氯苯基)-2-硝基环己酮的检验鉴定

本文通过高分辨质谱–液相色谱质谱联用（UHPLC-HRMS）、核磁共振（NMR）、傅里叶变换红外光谱（FTIR）等多种技术，对近期缴获的疑似毒品黄色粉末进行检验分析。将该样品主要成分的谱图与现有数据库比对后发现，该物质并不在数据库中。UHPLC-HRMS分析得到其精确分子质量和主要特征离子峰。通过比对特征离子峰，该物质与氯胺酮有较高的相似度。15N-NMR确定了硝基的存在；核磁分析确定了其化学结构，并对各峰进行了指认；IR确定了羰基、硝基、C–Cl化学键等官能团的存在。该黄色粉末确定为一种可被用于合成氯胺酮的新型前体2-(2-氯苯基)-2-硝基环己酮，为国内首次在疑似毒品中检出。氯胺酮在全球范围内滥用，中国已经进行管制，而其作为药用有其独特的优势，合成工艺在不断发展，制毒工厂可能采用新的制毒工艺而逃避监管，2-(2-氯苯基)-2-硝基环己酮可能为不法分子为逃避打击使用新的合成氯胺酮工艺中的重要前体。在缴获物中发现该物质为以后易制毒化学品的管制和相关案件的检验提供参考。     

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。     

胶体金免疫层析一步法快速检测G1m(3)因子

建立一种简便快速的胶体金免疫层析一步法 ,用于检测 G1m(3)因子。采用柠檬酸三钠还原法制备胶体金颗粒 ,标记抗人 G1m(3)单克隆抗体 ,研制出抗人 G1m(3)因子免疫层析检测试剂盒。样品的 G1m(3)因子 ,与测试条上的金标记抗体结合后沿着反应膜移动 ,再与膜上固相抗体结合形成肉眼可见的红色反应带。使用该方法可检出 10万倍稀释的血清样品 ,整个试验只需 5 min完成。对常见的 2 3种动物血 (痕 )检验 ,未出现交叉反应。在 10 0例样品的检测中 ,本方法的检测结果 ,与 Dot- EL ISA的检测结果的符合率为 10 0 %。该方法适用于法医物证快速检验。     

LC-MS/MS同时分析血液中五种巴比妥类药物

目的建立血液中巴比妥类药物液相色谱-串联质谱(LC-MS/MS)检测方法。方法血液中的巴比妥类药物用有机溶剂液-液萃取,以乙酰水杨酸为内标,LC-MS/MS测定。结果检测血液中五种巴比妥类药物的最小检出限(LOD)均为10ng/mL,线性范围在0.02￣10μg/mL内良好,方法的回收率70%￣87%。结论所建方法快速、灵敏、准确,可以满足临床毒物和法庭毒物分析的需要。     

Changed compounds of hydroxyzine in a human urine

During a forensic toxicological GC/MS screening, changed compounds of hydroxyzine were found in a man's urine taken about 20 h after ingesting sake (Japanese liquor) and tranquilizers. The structures of those compounds were assigned to 4-chlorodiphenylmethane(I), p-chlorbenzophenone(III), norchlorcyclizine(IV), 7-(p-chloro-alpha-phenylbenzyl)-2-hydroxy-2H,3H-oxazolo-[3,2 -alpha] piperazine(V), 1-(p-chloro-alpha-phenylbenzyl)-4-methylpiperazine-3-one(VI), N-(p-chloro-alpha-phenylbenzyl)-N'-formylmethyl-N'- hydroxyethyl-1,2-ethenediamine(VII) and 1-(p-chloro-alpha-phenylbenzyl)-4-[2-ethoxy(2-ethoxy)-ethyl] piperazine(VIII) on the basis of the fragmentation patterns and relative retention times except VIII which was identified using the synthesized compound. I, V, VI, VII and VIII have not been reported previously, but the possibility of metabolites of hydroxyzine is still uncertain.     

Embutramide,a Component of Tanax®(T‐61) as a New Drug of Abuse?

Tanax^®(T‐61) is a euthanasia solution commonly used in veterinary medicine in Europe. It consists of three active components: embutramide, mebezonium iodide, and tetracaine hydrochloride. Human consumption of Tanax^®(T‐61) is usually associated with suicide attempts. In our 15‐year‐long practice, embutramide was detected only three times but within a short period. First, it was found in the urine of a 42‐year‐old veterinarian, and the other two observations were made in a 16‐year‐old young man. Urine samples were analyzed using Shimadzu Prominence TOX.I.S.II. HPLC–DAD system with online SPE extraction system. Both of the two patients denied any intention to die. These cases show that this veterinary drug may also be considered as potential drugs of abuse.     

Child Abuse-Related Homicides in New Mexico: A 6-year Retrospective Review

Abstract:  We retrospectively reviewed autopsy records at a statewide medical examiner's office in order to identify and characterize deaths due to child abuse. In a 6-year period in New Mexico, the medical examiner investigated 45 deaths determined to be child abuse-related. Decedents were predominantly male (68.9%), Hispanic White (53.3%), and all were 5 years of age or younger, with a median age of 1 year. Head injuries were the most common cause of death (44.4%), followed by battered baby syndrome (15.6%). Relatives were involved as alleged perpetrators in 80% of the cases, with the father most often implicated (36.1% of cases), and 88.9% of child abuse injuries resulting in death occurred in the family's residence. Toxicology was positive in 26.7% of cases, but only two cases had substances of abuse present. Information on risk factors such as prematurity, parental age, and history of abuse was also collected.     

Simultaneous separation of different types of amphetamine and piperazine designer drugs by capillary electrophoresis with a chiral selector

The recent emergence of a new class of piperazine-type compounds has brought about the need for laboratory screening methods for both seized drugs and toxicological samples. These piperazine compounds, which include 1-benzylpiperazine (BZP) and 1-(3-trifluoromethylphenyl)piperazine (TFMPP), exhibit comparable physiological effects and can be substituted for the classic amphetamine-type drugs. We have optimized a chiral capillary electrophoresis (CE) separation that detects a set of 6 piperazine and 4 chiral amphetamine compounds in under 23 min using a 200 mM phosphate buffer at a pH = 2.8 with 20 mM hydroxypropyl- beta-cyclodextrin (HPbeta3CD). In addition to the above compounds, a series of "clandestine" BZP diHCl samples were also analyzed using this method to assess the ruggedness of the procedure. The novel CE separation was tailored to simultaneously detect these piperzine compounds in addition to amphetamine-type drugs. Distinct migration time and UV-spectral data were obtained for all compounds of interest.     

Spouse Abuse and Child Abuse by Army Soldiers

This study analyzed data collected by the U.S. Army’s Family Advocacy Program, the group primarily responsible for family violence prevention, identification, evaluation, treatment, and follow-up on Army installations. Patterns of spouse abuse and child abuse perpetrated within a five year period (2000–2004) were examined in a sample of 10,864 Army Soldiers who were substantiated for family violence offenses. Three groups of family violence offenders were compared: (1) those who perpetrated spouse offenses only; (2) those who perpetrated child offenses only; and (3) those who perpetrated both spouse and child offenses. Results showed that the majority of substantiated family violence offenders were spouse offenders who had not committed child abuse (61%), followed by child offenders who had not committed spouse abuse (27%), and finally those who committed both spouse and child offenses (12%). The three groups of family violence offenders differed in terms of the types of abuse they perpetrated (neglect of children, emotional abuse, physical abuse, and sexual abuse), their experiences of being a spouse abuse victim, and sociodemographic characteristics. Twelve percent of all spouse abusers committed multiple spouse abuse incidents, and 10% of all child abusers committed multiple child abuse incidents.     

Fatal Intoxications in a Forensic Autopsy Material from Epirus,Greece, During the Period 1998‐2010

In this retrospective study, we report the epidemiological characteristics of all poisoning deaths in Epirus, Greece, from 1998 to 2010; we present the toxicological findings and the statistical evaluation of the results. This is the first detailed scientific report on all the officially certified poisoning deaths concerning part of the Greek population. A total of 126 poisoning fatalities were recorded, 67 of them being mono‐intoxications (53.2%). The cause of poisoning was as follows: drugs of abuse (60%); carbon monoxide (19.8%); pesticides (9.5%); corrosives (4.8%); pharmaceuticals (4.8%); and spider bite (0.8%). The most frequently detected poisonous substances were as follows: heroin (65 cases), ethanol (55), benzodiazepines (42), carbon monoxide (25), cocaine (17), cannabinoids (17) and pesticides (12). Increasing tendency in poisoning death rates was recorded, due to an increase in accidental poisoning deaths attributed mainly to drugs of abuse (total, accidental, and drugs‐of‐abuse poisoning death rates per 100,000 inhabitants per year were 1.87, 1.19, and 0.79, respectively, in the period 1998–2002 and 3.97, 3.41, and 2.55, respectively, in the period 2007–2010).     

Substance Use and Intimate Violence Among Incarcerated Males

The purpose of this study was to examine substance use patterns among a sample of incarcerated males who report engaging in levels of intimate violence, as well as identifying similarities and differences in demographic, economic status, mental health, criminal justice involvement, relationships, and treatment factors for three groups of incarcerated males - those who report perpetrating low intimate violence, those who report perpetrating moderate intimate violence, and those who report perpetrating extreme intimate violence the year preceding their current incarceration. Findings indicated that low intimate violence group's perpetration consisted almost exclusively of emotional abuse. Moderately intimate violent males and extremely intimate violent males, however, report not only high rates of emotional abuse but physical abuse as well. The distinction between moderate and extremely violent groups was substantial. Findings also indicated that perpetrators at different levels of violence in this study did not vary significantly in age, employment history, marital status, or race. However, the three groups showed significant differences in three main areas: (1) cocaine and alcohol use patterns, (2) stranger violence perpetration and victimization experiences, and (3) emotional discomfort. Implications for substance abuse and mental health treatment interventions and for future research are discussed.     

Seizures of Clandestinely Produced Tablets in Santa Catarina,Brazil: The Increase in NPS from 2011 to 2017

Ecstasy is the name given to a large group of substances known as “club drugs” traded in the form of tablets, powder and liquid that present a varied composition, including mainly 3,4-methylenedioxymethamphetamine (MDMA) and analogous substances, in addition to the growing presence of new psychoactive substances. Based on this, clandestinely produced tablets (“ecstasy tablets”) seized by police in Santa Catarina in the period from 2011 to 2017 were analyzed. During the study period, 3472 seizures occurred, which resulted in total 498,443 tablets seized. Seventy nine substances were identified. In the year 2011, about 90% of the tablets contained MDMA. This number decreased to 66.6% in 2017. On the other hand, there was an increase in the number of tablets that mainly contained synthetic cathinones, as well as tryptamine and piperazine derivatives. Police seizures in the metropolitan region of Florianópolis and on the coast prevailed over the rest of the state.     

Fatal Oral Methylphenidate Intoxication with Postmortem Concentrations

Methylphenidate (MPD) is a widely prescribed stimulant used primarily for the treatment for attention‐deficit/hyperactivity disorder (ADHD). Suicide attempts involving MPD ingestion have been well described; however, deaths attributed solely to MPD ingestion have not been reported. A 62‐year‐old woman was found dead on her floor. The only discrepancy in among her medication quantities was that >three hundred 10 mg MPD tablets were missing. Analysis utilizing gas chromatography–mass spectrometry revealed elevated postmortem MPD peripheral and central blood, liver and vitreous humor concentrations. Considering both the central blood to peripheral blood ratio (0.89) and the liver to peripheral blood ratio (3.3), MPD does not appear subject to significant postmortem redistribution. With no other identifiable cause of death, we report what appears to be the first isolated MPD ingestion associated with a fatality.