LC／MS／MS法测定生物组织中百草枯

目的建立LC／MS／MS检测生物体液中百草枯方法。方法弱阳离子交换固相萃取小柱提取剂，应用LC／MS／MS法对生物样品中百草枯进行定性定量分析。结果经该方法测得百草枯的最小检出限为10ng／ml血（S／N≥3），线性范围为0．02～20μg／ml。结论该方法快速、灵敏、准确，适用于生物检材中百草枯的分析。     

Law/Holocaust/Academy

Book reviewed in this article:
Richard H. Weisberg, Vichy Law and the Holocaust in France     

Differentiation of side chain isomers of ring-substituted amphetamines using gas chromatography/infrared/mass spectrometry (GC/IR/MS).

Common analytical methods used for identifying samples obtained from clandestine laboratories were evaluated for their ability to differentiate between possible amphetamine isomers and homologs. A series of ring-substituted (4-methyl, 4-methoxy, and 3,4-methylenedioxy) amphetamine and N-methylphenethylamine isomers was analyzed using color tests, thin-layer chromatography, gas chromatography/mass spectrometry (GC/MS) and GC/infrared (GC/IR). The N-acetyl derivatives of the isomers were analyzed using GC/IR/MS. GC/IR/MS readily differentiated the 4-methylphenylalkylamine isomers. MS and IR spectra were also obtained for each pair of the 4-methoxyphenylalkylamine isomers and the 3,4-methylenedioxyphenylalkylamine isomers, but differentiation via GC/IR/MS was difficult. The N-acetyl derivatives of each pair of isomers could be readily differentiated using GC/IR/MS. Good library researchable spectra for N-acetylamphetamine could be obtained for IR identification with 10 ng (on-column) and MS identification with 2 ng. The spectrometrically independent IR and MS data obtained for the N-acetyl derivatives indicated that the combination of GC/IR/MS can add a significant level of confidence in the analysis of ring-substituted arylalkylamines.     

“连/又/一边A带/又/一边B”格式比较研究

连A带B"、"又A又B"和"一边A一边B"三种近义格式在形式、语义、语用方面都存在着明显的差异。在形式上,除音节的对称性和AB语法单位的不同外,三种格式A、B对动词性、形容词性、名词性成分的接纳所呈现的阶梯状分布差异,直接导致了三者句法功能的倾向以及格式义丰富性的差异。在语义上,前两种格式AB的概念关系关联度越高,越容易进入格式,后一种则相反;三种格式内部逻辑语义关系除都存在并列、顺承外,还都有着各自的特性。在语用上,"连A带B"和"又A又B"多表主客观的融合,而"一边A一边B"只表客观描写;三者焦点信息也不同:"连A带B"在A上,"一边A一边B"在B上,而"又A又B"的则在AB共同构成的语用意义上。     

Identification of selected psychopharmaceuticals and their metabolites in hair by LC/ESI-CID/MS and LC/MS/MS

Hair samples of patients of psychiatry and hair samples of suicide cases were analysed by liquid-chromatography/ionspray-mass spectrometry (LC/MS) for antidepressants and neuroleptics. Electrospray ionisation (ESI) with in-source collision induced dissociation (ESI/CID) and tandem-mass spectrometry (MS/MS) were used for drug and metabolite identification. Mass spectra library searching was performed using an ESI/CID mass spectra library and a MS/MS spectra library. Furthermore, extracted ion chromatograms were used for the detection of N-desmethyl-metabolites, which were also identified by their fragment-ion spectra. Three examples using these methods are shown: The tricyclic antidepressant maprotiline, the selective serotonin receptor inhibitor (SSRI) citalopram and their desmethylmetabolites as well as the neuroleptic pipamperone were detected and identified in hair extracts. For extraction powdered hair was treated by ultrasonication in methanol and solid-phase extraction was used for sample clean-up prior to LC/MS or MS/MS analysis. These examples demonstrate the power of LC/MS and LC/MS/MS for the detection and identification of drugs in hair extracts using full-scan mode and ESI/CID with library searching or using highly selective LC/MS/MS-analysis with library searching or in multiple reaction monitoring mode.     

南京话响音的鼻化度——兼论/n、l/不分的实质

本文使用鼻音计(Nasometer)考察了南京话响音的鼻化度。结果发现:南京话元音内在鼻化度大小与元音发音时舌位的前、后和高、低有关系,表现出与北京话大体一致的趋势,都是[a]的鼻化度最高,[u]的鼻化度最低,前高元音[y]的鼻化度也较低。元音的内在鼻化度及非鼻音浊声母[l]、[Z]的鼻化度在40以上,鼻音声母[m]的鼻化度在80以上,鼻化元音基本都处在N值40和80之间的断裂带上。南京话鼻音[n]与边音[l]相混的现象实质是/n/与/l/两个音位的完全合流,[n]与[l]是一个音位的两个条件变体,合流过程中产生了中介音——鼻化边音[I]。     

The cartography of responses to state crime: understanding the linkages among state abuses/crimes/deviance/harms/illegalities/wrongs,resistance/control,and state organizational reactions

Although a considerable amount of thoughtful scholarly research on state crime has been conducted and published, researchers have failed to assemble a comprehensive model of the process and reactions that begin after state crime has occurred and been detected. This article outlines a heuristic model that presents the major political actors that participate in this process and the relationships that can develop among them. In order to create the model, research that has been conducted on state crime is reviewed and integrated, difficulties with this work are analyzed, and recommendations about future research that can be conducted using the model are made.     

K?nig/Roeser/Stock: Baunutzungsverordnung

Ohne Zusammenfassung     

AGB-Kontrolle / Transparenzgebot / Begriff der "beiderseitigen Hauptleistungen" / Schriftformklauseln

Das Transparenzgebot des § 6 Abs 3 KSchG begnügt sich nicht mit formeller Textverst?ndlichkeit, sondern verlangt, dass Inhalt und Tragweite vorgefasster Vertragsklauseln für den Verbraucher durchschaubar sind. Vertragsbestimmungen müssen den Verbraucher im Rahmen des M?glichen und überschaubaren zuverl?ssigüber seine Rechte und Pflichten aus dem Vertrag informieren. Eine "gr?bliche Benachteiligung" iSv § 879 Abs 3 ABGB liegt vor, wenn die dem Vertragspartner zugedachte Rechtsposition in auffallendem, sachlich nicht zu rechtfertigendem Missverh?ltnis zur vergleichbaren Position des anderen steht. § 10 Abs 3 KSchG trifft nicht nur Klauseln, wonach mündliche Absprachen keine Gültigkeit haben, sondern insb auch solche, wonach ?nderungen und Erg?nzungen eines Vertrags nur durch eine schriftliche Best?tigung des Unternehmers wirksam sind. Zum Begriff der "beiderseitigen Hauptleistungen" iSv § 879 Abs 3 ABGB. Für die Kenntnisnahme der AGB durch den Verbraucher und die Zustimmung des Verbrauchers zu den AGB trifft den Unternehmer die Beweislast, sofern er sich auf die AGB beruft. Hat aber der Kunde bereits in den AGB best?tigt, dass er diese zur Kenntnis genommen und ihnen zugestimmt hat, wird ihm im Zuge der Rechtsverfolgung oder -verteidigung eine Beweislast auferlegt, die ihn von Gesetzes wegen nicht trifft, wenn er n?mlich nun seinerseits dartun muss, dass er ungeachtet der Best?tigung zB in Wahrheit gar keine M?glichkeit gehabt habe, die AGB zur Kenntnis zu nehmen.     

Analysis of drugs of abuse in hair by automated solid-phase extraction, GC/EI/MS and GC ion trap/CI/MS

In our laboratory, analysis of human hair for the detection of drugs of abuse was first performed in 1995. Initially, requests for hair analysis were few, and it is only since 1997 that these analyses have become routine. As demand grew, we developed an automatic solid-phase extraction method; the use of a robot ASPEC allowed us to drop certain fastidious manipulations, and to treat a large number of samples at a time. This method is described, along with analysis by gas-chromatography-mass spectrometry (GC/MS) in selected ion monitoring mode (SIM), for the following drugs: codeine, 6-monoacetylmorphine (6-MAM), morphine, cocaine, methadone, ecstasy (MDMA) and Eve (MDE). This requires prior derivatization with propionic anhydride. The different validation parameters, linearity, repeatability, recovery and detection limits are described, as well as the application of this method to some real cases. Analysis of these cases is also performed by an ion trap GC/MS in chemical ionization mode (GC/IT/CI/MS) in order to demonstrate the usefulness of this technique as a complement to routine analysis. Analysis by GC/IT/CI/MS indeed avoids the risk of false-positive results by the identification of metabolites.     

Haftung des Notars / Schadensverlagerung / Schadensminderungspflicht

Ein von der Grundstückseigentümerin beauftragter Notar, der versehentlich statt einer Teil- die Gesamtl?schung einer H?chstbetragshypothek beantragt, haftet wegen Verlustes der Pfandhaftung nicht nur der Hypothekargl?ubigerin, sondern auch einem Bürgen, auf den sich der Schaden durch die Uneinbringlichkeit seines Regressrechtes verlagert hat. Verletzt der Bürge seine Schadensminderungspflicht, weil er es im Rechtsstreit mit der Hypothekargl?ubigerin unterl?sst, den ihm durch Wegfall der Pfandhaftung entstandenen Schaden mittels entsprechender Einwendungen zu verhindern, führt dies zu einem Entfall der Haftung.     

SPME—GC／MS／MS法分析血中助燃剂残留物

目的探讨检验血中助燃剂残留物的分析方法。方法运用SPME(固相微萃取)技术,利用100μmPDMS萃取纤维,于室温条件下以顶空方式直接从血中萃取、浓缩挥发性碳氢化合物,用GC/MS/MS检测分析助燃剂。结果从检验的实际案例显示,可从0.1ml血中检出痕量的助燃剂。结论该方法操作时间短,检材用量少,分析结果较理想。     

GC/MS/AMDIS在法医毒物分析中的应用

目的探索自动质谱去卷积定性系统(AMDIS)在法医毒物分析中的应用。方法利用自动质谱去卷积定性系统(AMDIS)、全扫描离子模式(FIM)和选择离子监测技术(SIM)对农药、毒品、安眠镇静类药等常见毒物进行检索分析,比较三种检索方式对不同质量浓度(40.0、4.0、0.4mg/L)毒物的检验结果。结果AMDIS与SIM具有相近的灵敏度,可以将GC/MS全扫描文件去卷积处理,解决杂质干扰问题,准确对目标化合物进行定性;AMDIS可以自动识别重叠的色谱峰并将其与目标谱库进行匹配,为重叠峰的定性提供了直观的鉴别依据。结论AMDIS检索自动快速,适用于GC/MS法快速鉴定毒物。     

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.     

Academic/government/industry strategic research partnerships

Important factors for science to contribute to technological innovation are proper focus, scope, completeness, and timing. These are influenced by both the contexts and methodologies of research. In the context, there is a need to organize a bridging form between the sources of science and the implementors of technology. In the methodology, there is a need to adjust the approaches of science with the approaches of technological innovation. Cooperative research centers and next-generation-technology strategies have been shown to provide proper contexts and methodologies for coupling science with technology. National Science Foundation The opinions in this paper are solely those of the author and do not express official policy of the National Science Foundation.     

FTIR法检验海洛因中的淀粉、葡萄糖、蔗糖

目的建立检验掺有淀粉、葡萄糖、蔗糖的海洛因的新方法。方法红外光谱。结果给出了用FTIR检验掺有淀粉、葡萄糖、蔗糖的海洛因的判据。结论用红外光谱法可以准确、无损鉴定掺杂淀粉、葡萄糖、蔗糖的海洛因。     

固相微萃取（SPME）GC／MS、GC／MS／MS法检测环境水中的有机磷杀虫剂

目的　通过对固相微萃取 (SPME)条件的优化、筛选实验 ,建立环境水中有机磷杀虫剂的快速检验方法。方法　收集 17种有机磷杀虫剂 ,使用SPME并结合GC/MS、GC/MS/MS检验方法。结果　该方法简便、灵敏、迅速、可靠 ,样品利用率高 ,最低检测浓度为 0 .0 1～ 10 0 pg/ml,在痕量范围 0 .1～ 10ng/ml内线性回归好(相关系数r达 0 .99以上 )。结论　实际应用效果理想 ,有望成为公安、环保、检验检疫的农残及毒物分析中的一种快速有效的分析方法。