Application of discriminant analysis to differentiate between incorporation of cocaine and its congeners into hair and contamination

The requirement to differentiate between incorporation and external contamination of drugs into hair is undisputed, in particular when dealing with compounds which are administered by sniffing or inhalation (e.g. cocaine). With the aim of making this discrimination, hair samples from cocaine (COC) users (group IN) and seized cocaine samples (group OUT) were compared regarding the parameters benzoylecgonine (BZE), ecgonine methyl ester (EME), ecgonine (ECG), anhydroecgonine methyl ester (AEME), cocaethylene (CE) and norcocaine (NCOC). Since most of these compounds may be minor by-products of COC or be formed by biotransformation or chemical degradation, the stability of each substance was carefully examined. COC was found to be converted into significant amounts of BZE, EME and ECG even under mild extraction conditions, while traces of NCOC proved to be a ubiquitous by-product of COC. Cocaine positive hairs and seized cocaine samples (diluted to relevant concentrations) were equally preprocessed and analyzed by LC-MS-MS. Out of the metabolites listed above, NCOC, CE and AEME (each normalised to COC) were significantly increased in the incorporation group (i.e. hair samples from cocaine users). Based on this approach, a statistical discriminant analysis enabled us to make a prediction (and estimation of uncertainty) for each cocaine positive hair sample as to its likelihood of belonging to the group of cocaine users or of being contaminated.     

电感耦合等离子体质谱法测定金寨地区仿野生茯苓不同部位及其土壤中11种无机元素

目的 探究无机元素在金寨地区仿野生茯苓不同用药部位中的分布及在土壤中的富集特点。方法 采用微波消解法处理茯苓皮、白茯苓、赤茯苓及其菌核生长附近土壤,应用电感耦合等离子体质谱法测定茯苓不同部位及其土壤中K、Na、Mg、Fe、Mn、Zn、Cu、Se等11种无机元素含量。结果 金寨地区仿野生茯苓各部位元素分布有一定差异,大多数元素在茯苓皮中含量较高,茯苓不同部位总的无机元素含量从高至低顺序为茯苓皮、赤茯苓、白茯苓;茯苓不同部位对无机元素的吸收有选择性,但均以K、Fe、Mg、Na含量较高;茯苓不同部位对11种元素的富集系数存在差异,变化范围为0.005 2～0.782 3。结论 所建立的电感耦合等离子体质谱法简便、准确,适用于金寨地区仿野生茯苓不同部位及土壤中11种无机元素的含量测定。     

3个道地产区黄芪中钙、镁、锌、铁、铜、锰含量测定

目的 测定3个道地产区黄芪中钙(Ca)、镁(Mg)、锌(Zn)、铁(Fe)、铜(Cu)、锰(Mn)的含量,以探讨道地药材与微量元素的相关性。方法 采用硝酸-过氧化氢（体积比5〖DK〗∶2）体系微波消解黄芪样品,火焰原子吸收光谱法测定黄芪中Ca、Mg、Zn、Fe、Cu、Mn的含量。结果 内蒙古黄芪除Cu元素含量稍低于山西黄芪之外,Ca、Mg、Zn、Fe、Mn元素含量都高于甘肃黄芪和山西黄芪;山西黄芪除Zn元素含量不低于甘肃黄芪之外,Ca、Mg、Fe、Cu、Mn元素含量都低于甘肃黄芪。结论 在内蒙古、甘肃、山西3个道地产区黄芪中,人体必需微量元素含量以内蒙古黄芪最优,甘肃黄芪次之,山西黄芪再次之。     

气相色谱-质谱联用法分析 3种方法提取的三七挥发性成分

目的 运用气相色谱-质谱联用法对不同方法提取的三七挥发性成分进行比较分析。方法 分别采用回流提取法、超声提取法、静态顶空法提取三七挥发油,运用气相色谱-质谱联用技术,运用NIST11.0质谱数据库和峰面积归一化法对已分离的化合物进行鉴定并计算各成分的相对含量。结果 从回流提取、超声提取、静态顶空法提取的三七挥发油中分别鉴定出60、50、24个挥发性成分。在静态顶空法中相对质量分数最高的是香桧烯,占挥发性成分的24.97%;在回流提取法和超声提取法中相对质量分数最高的都是聚炔类物质环氧十三烷-4,11-二炔,分别占挥发性成分的9.97%和14.75%。首次从三七挥发性成分中鉴定出3个聚炔类化合物和2个甾体类化合物。结论 三七中挥发性成分主要为烷烃类、烯烃类、醛类、酸类、酯类、萜类、聚炔类、甾体类和杂环类物质。3种方法的补充利用可较全面地提取出三七中的挥发性物质。     

超高效液相色谱-四级杆飞行时间串联质谱快速分析复方守宫散化学成分及血中移行成分

目的 采用超高效液相色谱-四级杆飞行时间质谱(ultra-performance liquid chromatogra-phy/quadrupole time-of-flight-tandem mass spectrometry,UPLC-Q-TOF/MS)对复方守宫散中化学成分及其血中移行成分进行定性分析,为该制剂的...     

Identification of furosemide in hair in a post‐mortem case by UHPLC‐MS/MS with guidance on interpretation

Testing for drugs in hair raises several difficulties. Among them is the interpretation of the final concentration(s). In a post‐mortem case, analyses revealed the presence of furosemide (12 ng/mL) in femoral blood, although it was not part of the victim's treatment. The prosecutor requested our laboratory to undertake an additional analysis in hair to obtain information about the use of furosemide. A specific method was therefore developed and validated to identify and quantify furosemide in hair by UHPLC‐MS/MS. After decontamination of 30 mg of hair, incubation in acidic condition, extraction with ethyl acetate, the samples were analyzed by UHPLC‐MS/MS. Furosemide was found in the victim's hair at 225 pg/mg. However, it was not possible to interpret this concentration due to the absence of data in the literature. Therefore, the authors performed a controlled study in two parts. In order to establish the basis of interpretation, several volunteers were tested (four after a single 20 mg administration and twenty‐four under daily treatment). The first part indicated that a single dose is not detectable in hair using our method. The second part demonstrated concentrations ranging from 5 to 1110 pg/mg with no correlation between dosage and hair concentrations. The decedent's hair result was interpreted as repeated exposures. In the case of furosemide analysis, hair can provide information about its presence but cannot give information about dosage or frequency of use.     

用发射光谱分析测定电流斑中的金属元素

<正> 电流斑由肉眼或组织学观察有时难以确认,尤其是凶杀案件中,在电击死亡后,尸体经伪装或因腐败,从形态学确诊电流斑困难更大。因此,如能在可疑电流斑部位的皮肤组织中,检出接触皮肤导体的金属元素,对确认电击致死具有重要意义。作者结合两起案例,利用原子发射光谱分析法,对人体皮肤电流斑进行检验。现将结果报告于下。     

左归饮水提物对大鼠Cyp2b1、Cyp2c11、 Cyp2c7亚酶活性的影响

目的 采用Cocktail探针药物法评价左归饮对大鼠体内细胞色素氧化酶P450亚型酶Cyp2b1、Cyp2c11和Cyp2c7代谢活性的影响,为左归饮的开发应用提供实验依据。方法 选用阿莫地喹、安非他酮、奥美拉唑分别作为Cyp2b1、Cyp2c11和Cyp2c7的探针底物,制备成Cocktail混合溶液。将SD雄性大鼠分为实验组和空白组,实验组每日清晨灌服高、中、低剂量左归饮溶液,空白组每日清晨灌服空白溶剂,均连续给药14 d。第14天清晨尾静脉注射混合探针药物后于各时间点测定大鼠体内探针药物的血药浓度。经DAS 2.0软件计算探针药物的药物代谢动力学参数,评价左归饮对大鼠体内代谢酶活性的影响。采用LC-MS/MS法同时测定3种探针药物的血药浓度。结果 与空白组比较,高、中、低剂量左归饮连续给药对Cyp2b1、Cyp2c7和Cyp2c11酶活性的影响均无统计学意义（P＞0.05）。结论 左归饮配伍其他药物使用对代谢酶无明显影响,左归饮可在临床上广泛地配伍应用。     

中国节能减排的机遇与挑战

中国的节能减排亟需确立轻重缓急,权衡各种方案的利弊得失。它既要发挥市场的主体功能,又有赖于政府宏观调控弥补市场缺陷;既要确保经济增长活力,又要兼顾生态环境的保护;既要努力提高传统能源的利用效率,又要为潜在的新能源变革做好准备;既要承担国际责任,又要维护中国的发展空间。     

Acute arsenic poisoning: clinical, toxicological, histopathological, and forensic features

This report describes a suicide case by acute arsenic intoxication via intravenous injection. A 30-year-old woman injected arsenic As (V) (sodium arseniate disodique: Disodium Hydrogena Arsenik RP) in a successful suicide attempt. Three hours following administration, the woman developed severe digestive symptoms. She was admitted to a hospital and transferred to the intensive care unit within 12 h of the massive administration of arsenic. Despite therapeutic efforts, over the next 2 h she developed multiorgan failure and died. A postmortem examination was performed. Pulmonary edema and congestion of liver were apparent. As (V) and As (III) were determined by high performance liquid chromatography and inductively coupled plasma mass spectrometry after mineralization of samples by concentrated nitric acid. Toxicological analysis revealed high concentrations of arsenic in biological fluids as well as in organs. Histopathological examination showed a typical indication of myocarditis. These findings were in agreement with acute arsenic poisoning. The symptoms developed by this young woman (intoxication by intravenous administration) were comparable to oral intoxication. The clinical signs, survival time, and administration type are discussed in light of the literature on acute and chronic arsenic poisoning.