铁灭克的检验

目的建立生物检材中铁灭克农药的定性、定量分析方法;方法利用溶剂苯萃取生物检材中的铁灭克农药,应用薄层色谱(TLC)、气相色谱(GC)两种方法进行定性分析,应用气相色谱-质谱-选择离子监测(GC-MS-SIM)分析方法进行定性定量分析,并测定了该方法的检测限、线性回归方程和回收率。结果应用TLC、GC、GC-MS、GC-MS-SIM等分析方法成功地在两个实际案例中检出了铁灭克农药,利用GC-MS联用技术获得了铁灭克热解产物涕灭威腈的质谱图,GC-MS-SIM分析方法分析涕灭威的检测限是0.02ng,获得了m/z68、m/z100和m/z115三个特征离子定量分析的线性回归方程,样品添加标样回收率为99.0至103.5%。结论铁灭克热不稳定,受热易分解。获得了铁灭克热分解产物涕灭威腈的质谱图。GC-MS-SIM分析方法检测铁灭克具有灵敏度高、回收率高等优点。     

SPE-GC／MS检测生物样品中利多卡因、罗哌卡因、布比卡因

目的建立生物样品中利多卡因、罗哌卡因、布比卡因的固相萃取提取方法和气质检测方法。方法采用Oasis HLB固相萃取柱,以GC／MS定性定量。结果生物样品中利多卡因、罗哌卡因、布比卡因平均萃取回收率达74％以上,检测限0．01μg／mL,线性关系良好,相关系数R2=0．9900以上。结论方法操作简便快速,萃取回收率高,重现性好,可用于实际案件。     

硼氢化钠氯化镍还原-GC／TSD法检测血液和尿液中百草枯

目的 建立血液和尿液中百草枯的还原反应-GC/TSD分析方法.方法 生物样品经氯化钠盐酸溶液与氯仿-乙醇混合溶液去除蛋白后,上清液中目标物用硼氢化钠/氯化镍还原.乙酸乙酯提取.GC/TSD-热离子检测器分析.乙基百草枯为内标.结果 血液和尿液中百草枯检测限(S/N=3)分别为0.002和0.004μg/mL;线性范围0.050-30.0μg/mL,相关系数r分别为0.999和0.998,方法回收率均大于80%.结论 本方法准确、灵敏,重现性好,适用于体液中百草枯的检测.     

顶空气相色谱法检测生物检材中乙醇及其相关物质

目的建立生物检材中乙醇及其相关物质的检测方法。方法生物检材加入内标异丙醇后用顶空气相色谱法进行检测(FID检测器),以保留时间定性,内标法定量。结果该方法线性范围为0.05035～1.613mg/ml,相关系数r=0.9999,最低检测限(limit of detection,LOD)为3.379μg/ml,分析方法平均回收率为98.24%～106.5%,日内精密度RSD<2.2%,日间精密度RSD<1.4%,总分析时间不超过18min。结论该方法可用于生物检材中乙醇及其相关物质的检测。     

生物检材中苯丙胺类兴奋剂和氯胺酮的LC-MS/MS分析

目的建立生物检材中苯丙胺类兴奋剂和氯胺酮的液相色谱-串联质谱(LC-MS/MS)分析方法。方法生物检材包括血液、尿液和毛发,采用稀释法和液液提取的前处理方法,应用两个不同的液相柱,优化LC-MS/MS分析方法,并考察了血液和尿液基质的离子抑制作用。结果同时分析苯丙胺和MDA,液相1在3m in内完成,液相2可用于确认分析或复杂基质分离。尿液稀释法检材用量少,前处理简便快速。毛发中苯丙胺类兴奋剂和氯胺酮的最低检测限(LOD)为0.005~0.05ng/mg。对送检案例检材产妇头发和胎毛进行苯丙胺类兴奋剂和氯胺酮的分析。结论本方法可用于生物检材中苯丙胺类兴奋剂和氯胺酮的同时分析,血、尿等生物检材的离子抑制作用是影响本方法灵敏度的主要原因。     

固相提取净化生物试样中巴比妥类药物的研究

本文研究了用国产GDX-403固相柱提取生物试样中6种常见巴比妥类药物和GC/NPD分析方法。以血和肝为样本,分别添加2.0μg和5.0μg6种混合药物,在pH分别为6.0和2.2时对样品进行富集与净化,经GC/NPD分析,各实验药物回收率平均≥80％,方法变异系数为±0.1。建立的方法具有快速、灵敏、可靠的特点,在法医毒物分析中应用效果良好。     

生物检材中吗啡类生物碱的LC-MS／MS分析

目的针对滥用药物分析鉴定实践中亟待解决的问题,开展LC-MS/MS分析生物检材中吗啡类生物碱的应用研究。方法满足不同的鉴定需要,分别建立血液、尿液、唾液和头发等生物检材的样品前处理方法,确定同时分析海洛因、单乙酰吗啡、吗啡、可待因、乙酰可待因、二氢可待因酮和氢吗啡酮等吗啡类生物碱的LC-MS/MS方法。将方法应用于实际案例。结果所建立的方法对吗啡类生物碱分离良好。尿液稀释法、尿液提取法和头发中吗啡的最低检测限(LOD)分别为10ng/mL、0.01ng/mL和0.01ng/mg。结论所建立的方法简便、快速、特异性强、灵敏度高。目标物中加入二氢可待因酮和氢吗啡酮扩大了方法的实用范围。     

顶空气相色谱法检测生物检材中乙醇及其相关物质

目的建立生物检材中乙醇及其相关物质的检测方法。方法生物检材加入内标异丙醇后用顶空气相色谱法进行检测（FID检测器）,以保留时间定性,内标法定量。结果该方法线性范围为0．05035-1．613mg／ml。相关系数r=0．9999,最低检测限（limit of detection,LOD）3．379μg／ml,分析方法平均回收率为98．24％～106．5％,日内精密度RSD〈2．2％,日间精密度RSD〈1．4％,总分析时间不超过18min。结论该方法可用于生物检材中乙醇及其相关物质的检测。     

液化石油气中毒生物组织检验初探

<正> 近年来,液化石油气做为家庭燃料,使用越来越广泛。随之而来的意外中毒、自杀、谋杀等案件时有发生。而有关生物组织中的液化石油气的检验国内还未见报道。笔者在参考国外有关文献资料的基础上进行实验,建立了用顶空气相色谱法测定生物样品中石油液化气成份的分析方法,现报告如下。     

毒性元素砷、汞、铅试样处理方法及等离子体光谱测试技术研究

本文详细地介绍了低温加压消化法处理生物样品中毒性元素砷、汞、铅的处理方法.研究表明样品处理回收率为92%～95%,检测灵敏度达 ppb级,相对标准偏差系数<2%.建立了一个适用于从痕量到高含量砷、汞、铅检材的毒化标准分析方法.结果表明该法灵敏度高、准确、简便、快速,对砷、汞、铅的检验水平提高到了国内最高水平.     

GC-MS determination of gamma-hydroxybutyric acid (GHB) in blood

A fast and efficient procedure has been developed for the analysis of total mercury in human tissues and blood using a hydride vapor generator system coupled to an atomic absorption spectrometer (HVG-AA). Tissue and blood samples were digested in a pressurized microwave decomposition system and the digest diluted prior to formation of free mercury vapor and analysis by atomic absorption. Recovery studies performed on 10 spiked/unspiked pairs of human liver and on 10 spiked/unspiked pairs of human blood samples yielded average recoveries of 99.7% (CV=0.4%) and 101.2% (CV=0.5%), respectively. The method detection limit for liver and blood was 50 microg Hg/kg and 12.5 microg Hg/l, respectively. The "normal" concentrations of mercury in human liver and blood are 33-490 microg Hg/kg and 0.6-59 microg Hg/l, respectively [1]. This method is able to determine mercury poisoning levels and may also be applied to detect mercury near the lower levels of these "normal" ranges, using the standard addition method approach.     

Determination of ethyl glucuronide in human hair by SPE and LC-MS/MS

A method for the sensitive and selective determination of ethyl glucuronide (EtG) in hair has been developed using solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Washed and cut hair segments were extracted by ultrasonication (3h, 50 degrees C) and the extracts were cleaned-up with aminopropyl SPE columns. LC-MS/MS analysis was performed using a polar-endcapped phenyl-hexyl-RP-phase with negative mode electrospray ionisation (ESI) using a triple quadrupole mass spectrometer (Sciex API 365) with a turboionspray source and post-column addition of acetonitrile for enhanced sensitivity. The MS/MS transitions monitored were m/z 221 -->75 for EtG and 226 -->75 for D(5)-EtG as an internal standard. The method was selective and sensitive, with a detection limit of 51 pg/mg hair at a signal-to-noise ratio of 3:1. The mean recovery was 96%, with an intra- and inter-day precision of less than 11.7% at a concentration of 200 pg/mg. The linearity was assessed in the range of 25-2000 pg/mg hair, with a correlation coefficient of 0.997. The method was successfully applied to 97 human hair samples which were taken at autopsies from persons with known alcoholism or were obtained from alcoholics who were hospitalized for ethanol withdrawal, from social drinkers and from children having not consumed any alcohol. Although, approximately two-third of the alcoholics showed EtG concentrations in hair of higher than 51 pg/mg (up to >4000 pg/mg), in one-third the EtG concentration was below the detection limit. However, only in one of five hair samples of "social drinkers", the EtG concentration was above the detection limit (51 pg/mg). No EtG has been detected in the hair of children. These investigations demonstrate that heavy alcohol consumption may be but not necessarily has to be detectable by EtG analysis in hair.     

UFLC法测定新型“spike99”香料中JWH-073的含量

目的 超快速液相色谱法测定新型“spike99”香料中JWH-073的含量.方法 采用Shim-pack XR-ODSⅡ色谱柱(2.0mm×75mm,2.2μm);流动相:乙腈(含0.1％甲酸):水(含0.1％甲酸)(80∶20,v/v),流速:0.25 mL/min;检测波长280nm,柱温:35℃,进样量:2μL,外标法定量测定JWH-073的含量.考查方法的线性范围、灵敏度、精密度、回收率和稳定性,并用于检测实际案例样品.结果 JWH-073浓度在1～50μg/mL范围内线性良好(A=9 398.7C-635.75,r =0.999 9);最低检测限为100ng/mL(S/N=3);低、中、高3种浓度的加样回收率(n=3)分别为100.52％(RSD=0.36％),99.52％(RSD =0.43％),99.03％(RSD =0.17％).结论 本法测定新型“spike99”香料中JWH-073含量操作简便、灵敏、准确,重复性好,适于在相关案件检验中选用.     

Identification and characterization of the new designer drug 4'-methylethcathinone (4-MEC) and elaboration of a novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method for seven different methcathinone analogs

A fast and simple LC-MS/MS method was developed for screening mephedrone, butylone, methylenedioxypyrovalerone (MDPV), flephedrone, methylone and methedrone in bulk powder samples. Samples were separated on a reverse phase column using gradient elution with mixtures of water, acetonitrile and formic acid. After optimization a limit of detection of about 2ngmL(-1) was achieved using multiple reaction monitoring (MRM) mode. Total run time was less than 8min. Typical fragmentation characteristics of the studied compounds are discussed. The method was successfully applied to several unknown bulk powder samples seized by the Hungarian Customs and Finance Guard. One of the samples contained the new designer drug 4'-methylethcathinone (4-MEC), which was identified and characterized by LC-MS/MS, NMR, FT-IR and LC-TOF-MS techniques. The method is also deemed to be applicable for the screening of simple dosage forms such as tablets and capsules.     

中国个人信息保护法草案若干问题

在个人信息保护法草案中,个人信息的定义应修改为"个人信息是能够单独或者与其他信息结合识别有生命的自然人的各种信息,不包括匿名化处理后的信息."并加一款体现"识别"+"关联"的立法思路的文字.个人信息处理的列名操作应该由七个变更为十一个,即收集、存储、加工、使用、交易、提供、公开、查阅、复制、更正、删除等.第六十九条匿名...     

中国农村金融成熟度测量与研究

随着"软件能力成熟度模型"(CMM)的完善,"成熟度"这一概念在很多领域得到了广泛应用.将"成熟度"的概念引入金融发展领域,形成"金融成熟度"及其指标体系和测算方法,再采用主成分分析方法对我国9个省级地区的农村金融成熟度进行测量并排序.结果表明,我国农村金融发展呈现区域发展不平衡的局面,东部地区处于领先地位,发达省区如浙江的农村非正规金融活动盛行.因此,对发达地区农村非正规金融应加强引导和监管;对欠发达地区农村金融发展,既要给予一定的政策倾斜,更要注重改善其涉农基本制度.     

Methadone extraction from minimal amounts of biological fluids

A new solid phase extraction method was studied to extract methadone from small amounts of biological samples, by using little disposable columns prepacked with reverse phase sorbents. Two different commercial kinds of reversed phase columns prepacked with octadecylsilane (ODS) were tested; the results were compared to those obtained by a direct liquid/liquid extraction method. Gas chromatograms of extracts obtained by means of ODS reversed phase columns showed a good signal/noise ratio resulting in higher sensitivity (20 ng/ml as detection limit), in comparison with the liquid/liquid extraction method.     

Determination of gamma-hydroxybutyrate in water and human urine by solid phase microextraction-gas chromatography/quadrupole ion trap spectrometry

A simple method of detection was developed for gamma-hydroxybutyrate (GHB). The method involves the derivatization of GHB using a hexyl-chloroformate procedure in aqueous media (such as water or urine), extraction of the derivatization product directly from the sample using solid-phase microextraction, and subsequent separation and detection with gas chromatography quadrupole ion trap mass spectrometry. The deuterated form of GHB (GHB-D6) is used as an internal standard for quantitation. The method was linear for GHB-spiked pure water samples from 2 to 150 microg/mL GHB with a detection limit of 0.2 microg/mL. Spiked urine samples showed linearity from 5 to 500 microg/mL GHB with a detection limit of 2 microg/mL. The SPME-GC/MS method is applied to actual case samples, and the results are compared to those values obtained using a conventional GC/MS method. Sensitivity and linearity are comparable to those seen using traditional methods of separation, yet the SPME method is superior due to the simplicity, speed of analysis, reduction in solvent waste, and ability to differentiate between GHB and gamma-butyrolactone (GBL).     

The use of amalgam powder and calcium hydroxide to recreate a radiopaque image of a lost dental restoration

Radiographs of dental restorations are highly reliable when used to identify postmortem dental remains. A problem exists if key dental restorations are missing or defective, which results in the loss of a comparative radiographic image. This article describes a simple method allowing the odontologist to quickly recreate a temporary radiopaque restoration. This article presents a method of using amalgam powder (radiopaque material) and calcium hydroxide (radiopaque material and transport medium for the amalgam powder) to recreate a radiopaque image on a tooth that has lost a dental restoration. Amalgam powder and calcium hydroxide is easily obtained (in any dental office), fairly clean, easy to manipulate, inexpensive, inert, stable, and able to be removed without damaging the dental remains. The amalgam powder/calcium hydroxide mixture can easily be re-shaped or modified to reflect the radiopaque image of the original restoration. Radiographic comparison of the "restored" dental remains to the antemortem radiographs is now possible. The use of this technique is presented in a case report.     

Evaluation of 5-(4-nitrophenyl)-2,4-pentadien-1-al (NPPD) as a tracer for shadowing pursuits

The chemical compound 5-(4-nitrophenyl)-2,4-pentadien-1-al (NPPD), called "spy dust," was used in the Soviet Union as a shadowing pursuit, the act of following someone secretly, for investigating the activities of diplomatic personnel. It is also useful for counter-terrorism, and some criminal cases in the forensic science field. In this paper, it was synthesized and evaluated as a tracer for shadowing pursuits. The method for utilizing this reagent was very simple: it was dissolved in methanol (1 mg/mL) and sprayed on the restricted area. If the suspect was to enter this area or touched the sprayed material, NPPD was attached to the suspect's shoe surface or hands. The color examination was a two-steps process: first was the addition of 1 mL of a 0.1% naphthoresorcinol methanol solution to the methanol extracts of a methanol-contained cotton swab used to smear some surfaces of the suspect, and second, the addition of 1 mL of concentrated hydrochloric acid, which turned the solution dark red. The gamma max of the colored solution was 510 nm, measured by ultraviolet-vis spectroscopy. Detection limits for three methods were determined: a visual method (detection limit 100 ng/3 mL), an ultraviolet-visible spectrometric method (detection limit 10 ng/3 mL), and a selected-ion-monitoring gas chromatographic/mass spectrometric method (detection limit 300 pg/injection). The forensic utility of NPPD was demonstrated for two simulated cases: a theft case and a case where NPPD was used as a tracer to prove that an automobile had entered a restricted area. These examinations prove NPPD is a useful shadowing pursuit (spy dust) for the forensic science field.