一些常见药物在ODS柱上的分离

应用高效液相色谱技术,进行药物的分离、分析已有很多报导。为了在尽可能简便的条件下.较为有效地进行一些药物,主要是弱极性结构药物的初步判断,我们采用 ODS 柱做了些探索。对于一些常见药物,如巴比妥类、安定类、解热镇痛类及某些抗菌素类药物均能观察到较为满意的分离效果。     

Observations on the specificity of breath-alcohol analyzers used for clinical and medicolegal purposes

This paper deals with the application of three kinds of breath-alcohol analyzer for clinical and medicolegal purposes. The limited specificity for analyzing ethanol in expired breath has given misleading information with potential serious consequences. Three different methods of alcohol analysis are reported: semiconductor sensing (Alcotest 7310), electrochemical fuel cell (Alcolmeter SM-1), and infrared (IR) absorptiometry (IR Intoximeter 3000). Methanol could not be distinguished from ethanol with any of these breath-test instruments. When nonspecific techniques of ethanol analysis are used, the results must be considered with caution when interfering substances expelled in breath cannot be excluded.     

A novel method for extraction and analysis of gunpowder residues on double-side adhesive coated stubs

A study was conducted to develop an efficient method for extraction and analysis of gunpowder (propellant) residues from double-side adhesive coated stubs, which are used for sampling suspects or their clothing for gunshot (primer) residues (GSR). Conductive and non-conductive double-side adhesives were examined, and the analysis was carried out by gas chromatography/thermal energy analyzer (GC/TEA) and ion mobility spectrometry (IMS). The optimal procedure for the extraction, as was developed in the present study, employs two stages: (1) extraction of the stubs with a mixture of 80% v/v aqueous solution of 0.1% w/v of sodium azide and 20% v/v of ethanol employing sonication at 80 degrees C for 15 min. and (2) residues from the obtained extract were further extracted with methylene chloride. The methylene chloride phase was concentrated by evaporation prior to analysis. Extraction efficiencies of 30-90% for nitroglycerine (NG) and for 2,4-dinitro toluene (2,4-DNT) were found. No significant interferences in the analysis were observed from the adhesives or skin. Interferences were observed in the analysis by the GC/TEA of the samples collected from hair. The method enables analysis of propellant residues on a double-side adhesive coated stub after it was examined for primer residues by scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDX). Thus, the probative value of the evidence may be increased.     

Concentration-time profiles of ethanol in capillary blood after ingestion of beer.

Blood ethanol profiles were determined in experiments with healthy volunteers after they had drunk beer. When 330 ml of light beer (1.8% w/v ethanol) was consumed in 5 min by four men and four women, the average peak blood-alcohol concentration (BAC) reached was 8 mg/100 ml (range 2-11). After nine men had drunk 660 ml of beer (3.0% w/v or 3.6% w/v ethanol) in 25 minutes on an empty stomach, the average peak BAC was 32 mg/100 ml (range 26-44) and 37 mg/100 ml (range 23-54) respectively. When the same two beers were consumed by another nine men together with a meal, the peak BAC was 24 mg/100 ml (range 20-29) and 28 mg/100 ml (range 20-39) respectively. The peak BAC occurred earlier when beer was ingested together with food; mean 32 min (range 30-50) compared with 41 min (range 30-70) with an empty stomach. The rate of disappearance of alcohol from blood (beta-slope) was 12 mg/100 ml/h in the fed state and 15 mg/100 ml/h when subjects were fasted. The apparent volume of distribution of ethanol (Vd) was 0.65 l/kg (SD 0.07) for the empty stomach condition but exceeded unity when beer was ingested together with food. It seems that part of the dose of alcohol when consumed with food never reaches the systemic circulation.     

Effect of eight solvents on ethanol analysis by Dräger 7110 Evidential breath analyzer

The Dr?ger 7110 MK III FIN Evidential breath analyzer is classified as a quantitative analyzer capable to provide sufficient evidence for establishing legal intoxication. The purpose of this study was to evaluate ethanol specificity of this instrument in the presence of other solvents. Effects of eight possible interfering compounds on ethanol analysis were determined in a procedure simulating a human breathing. Most of the compounds studied had either a negligible effect on ethanol analysis (acetone, methyl ethyl ketone, and methyl isobutyl ketone) or were detected in very low concentrations before influencing ethanol readings (methanol, ethyl acetate, and diethyl ether). However, 1-propanol and 2-propanol increased the ethanol readings significantly. Thus, Dr?ger ethanol readings should be interpreted carefully in the presence of propanol.     

Effect of ethanol on cardiac single sodium channel gating

Alcohol in modest and higher doses has the potential to induce cardiac arrhythmias. The most famous alcohol-related arrhythmia is the "holiday heart syndrome". Furthermore, there is a clear association between excessive alcohol consumption and the risk of sudden cardiac death. However, the acute effects of ethanol on arrhythmia induction are not well understood. The effect of ethanol on single cardiac sodium channels has not been studied yet. To elucidate the effect of ethanol on human cardiac sodium channels we performed a patch clamp study in HEK-293 cells overexpressing the human cardiac sodium channel. We used HEK-293 cells overexpressing the human cardiac sodium channel (Na(1.5)). Single channel gating was investigated by the cell-attached patch clamp technique. Sodium channel currents were elicited by depolarizing pulses from -120 to -20mV for a duration of 150ms. Single channel availability, open probability and peak average current were assessed baseline and after addition of ethanol in increasing concentrations (0.50 per thousand (10.9mM), 1.00 per thousand (21.7mM), 2.00 per thousand (43.5mM) and 4.00 per thousand (87.0mM)). We found a concentration-dependent reduction of open probability which was statistically significant at 2.00 per thousand ethanol (66.5+/-14% of control). At higher concentrations (4.00 per thousand) also availability decreased to 66.5+/-11.0% of control. This resulted in a significant decrease of peak average current at 2.00 per thousand and at 4.00 per thousand ethanol (61.8+/-7.4 and 53.0+/-8.2% of control). For the first time the present study demonstrates acute inhibitory effects of ethanol on single cardiac sodium channel gating and provides one potential mechanism for the well known clinical observation that ethanol triggers supraventricular and ventricular arrhythmias.     

About the effect of alcohol and tiredness on the activity of tendon reflexes (author's transl)]

In order to estimate the combined effect of ethanol and fatigue on the activity of tendon reflexes, the mechanical threshhold and the latency of the patellar tendon, the radial and the biceps reflexes as well as the time of contraction of the musculus quadriceps femoris was investigated in men, with an ethanol level in blood at 80 mg % during elimination-period, and with tired subjects meaning that they hade done their usual daywork and had been awake for about 20 to 22 hours. The group, consisting of 21 male students, was then investigated under both these conditions. The patellar reflex was elicited by a specially constructed reflexhammer, by which the mechanical power could by measured exactly, from the angle of the position the hammer was released from and its known weight. The latency and the muscular contraction time were registered with electrodes on the skin by an oscillograph. The mechanical threshhold of the patellar, biceps and radial reflexes and the latency of there reflexes were significantly and equally impaired by ethanol as well as by fatigue. The combination of both these factors resulted in an almost exactly additional effect. The contractiontime of the m. quadriceps was prolonged more by fatigue than by ethanol. Comparing these results with fromer findings, a depressing effect of the formatio reticularis of the brainstem on the activity of the spinal motorcells is to be discussed. This impairment of neuro-muscular coordination and activity obviously is dangerous for drivers. It should especially be noted, that the effect of a wake period of 20 to 22 hours can be compared with that of a bloodlevel of 80 mg % ethanol as to the impairment of the tendon reflexes.     

Medicolegal studies on alcohol detected in dead bodies — alcohol levels in skeletal muscle

An experiment was carried out on rats to determine whether or not a skeletal muscle sample was suitable for the determination of ethanol concentration in a carcass. Gas chromatography was used to estimate the ethanol and n-propanol concentrations in the femoral muscle and intracardial blood. The ethanol concentration of each sample was corrected according to the moisture ratio of circulating blood, viz., 78.5%.The ethanol concentration ratio of blood to muscle was 1.03 two hours after ethanol administration. When the carcasses of rats pre-treated with ethanol were stored at 15 °C and 25 °C, respectively, the ethanol concentrations in muscle and blood increased with time. At all times the concentration was higher in blood than in muscle, and also higher in samples collected from the carcass stored at 25 °C than at 15 °C.When the control carcass was stored in the same manner, the postmortem production of ethanol was noticed in both blood and muscle. As in the experimental rats, the control rats exhibited a higher blood ethanol than muscle ethanol level. Again, the ethanol concentration was higher in samples collected from the carcass stored at 25 °C than at 15 °C. The ratio of ethanol to n-propanol was less than 20:1 in blood and less than 10.1 in muscle.These results suggest that skeletal muscle may be a suitable tissue for the postmortem detection of ethanol.     

Ballistic skin simulant

Hydrogels prepared from water solutions containing 10-20 mass% gelatine are generally accepted muscle tissue simulants in terminal ballistic research. They, however, do not have a surface layer which simulates the effect of human skin. The purpose of this research was to find a suitable skin simulant for enhancing the testing fidelity and the credibility of the results with gelatine-based materials when assessing the injury potential of not only high energy bullets, but also especially that of non-penetrating "less lethal" kinetic impact ammunition and relatively low energy ricochet fragments. A skin simulant also permits the simulation and assessment of exit wounds. The mechanical and ballistic properties of human skin and target simulant were established on the basis of results found in the literature. Some errors in these were found. The corrected values are included in this paper for comparison. The target values of the mechanical properties of the skin simulant were the following: threshold velocity v(th)=94+/-4 m/s, tensile strength 18+/-2 N/mm2 and elongation at break 65+/-5%. A selection of synthetic and natural materials was evaluated as skin simulants by analysing their mechanical and ballistic properties. The results were compared to literature values obtained with human cadavers. The tests showed that the best skin simulant of the ones evaluated was semi-finished chrome tanned upholstery "crust" cowhide of 0.9-1.1 mm nominal thickness. Its threshold velocity was 90.7 m/s, tensile strength 20.89+/-4.11 MPa and elongation at break 61+/-9%. These values are the same as the average values of human skin. Of the synthetic materials evaluated, 1mm thick natural rubber can be used on impact side as a threshold velocity filter with some reservations although its theoretical threshold velocity is only 82.9 m/s.     

DNA数据库建设中批量样品不同DNA提取方法的比较

目的比较和选择自动化工作平台提取DNA的方法,并用于DNA数据库建设。方法用手工Chelex-100法、Biomek3000自动化工作平台结合Chelex-100法及DNA-IQTM磁珠法对实验室收集的建库滤纸血样进行DNA提取,荧光定量技术对上述3种方法提取的模板DNA进行测定;扩增产物用3100基因分析仪检测并用基因分析软件分析。结果手工Chelex-100法、自动化Chelex-100法及DNA-IQTM磁珠法提取的DNA模板浓度分别为0.593ng±0.131ng/μl、0.579ng±0.096ng/μl、0.447ng±0.056ng/μl;成功率分别为100%、98.9%、99.5%。结论本文建立的自动化Chelex-100法可用于大规模DNA数据库建设。     

Differences between multisite postmortem ethanol concentrations as related to agonal events

In a study of postmortem ethanol concentrations, blood was withdrawn from the right atrium, ascending aorta, and inferior vena cava. These samples, vitreous humor, and gastric fluid were analyzed in 307 autopsies, where a minimum blood ethanol concentration of 0.05% weight/volume (w/v) was present. Premortem, agonal, and postmortem events were reviewed in an attempt to account for differences in blood ethanol concentrations between sites. The agonal aspiration of vomitus having at least 0.80% w/v ethanol appears to be associated with an increase in aortic ethanol concentrations. We conclude that valid interpretation of postmortem ethanol concentrations must take into consideration the possible entry of ethanol into the pulmonary venous circulation via the respiratory system.     

Delayed ethanol analysis of breath specimens: long-term field experience with commercial silica gel tubes and breathalyzer collection

Delayed ethanol analysis was performed on breath specimens collected with commercial silica gel tubes using multiple Breathalyzer instruments. Eleven hundred and nine results were obtained from an ethanol testing program over a five-year period. Only 2.5% of the specimens had apparent collection errors. For the valid specimens, the most frequent result was 0.11 g/210 L and the mean result was 0.14 g/210 L. For 642 specimens, delayed results were compared with direct results. Direct results were greater than delayed results for 55%, less than for 27%, and equal to for 18% of the pairs. When fixed tolerance limits of +/- 0.03 were used, 81% of the direct results were confirmed. The confirmation percentage was best in the critical range of direct results, 0.05 to 0.15 g/210 L. The collection tubes showed no substantial variability in retaining ethanol during storage and releasing ethanol for analysis.     

Comparison of Different Swabs for Sampling Inorganic Gunshot Residue from Gunshot Wounds: Applicability and Reliability for the Determination of Firing Distance

This study concentrates on samples of bare pork skin, with and without bristles, and dried bovine ribs shot with a semi‐automatic pistol to find the best methodology and sampling surface in the search for inorganic gunshot residues (IGSR). Four quadrants of known surface areas were sampled at different distances from the bullet's hole with different swabs: tapes in graphite, Leukosilk® white tape, 3M® transparent tape, and a cotton swab to assess the technique able to collect the highest amounts of IGSR with the lowest contribution of the blank. The cotton swab wet in 10% HNO₃ gave the best results. The highest amounts of IGSR, measured by ICP‐OES and MS, were detected on a surface of 3‐cm radius from the bullet's edge. The amount of metals collected decreased with the firing distance between 20 and 60 cm. The procedure was efficient for sampling different tissues like skin and bones.     

Fourier-transformed infrared breath testing after ingestion of technical alcohol

The study aim was to evaluate the feasibility of a Fourier-transformed infrared (FT-IR) analyzer for out-of-laboratory use by screening the exhalations of inebriated individuals, and to determine analysis quality using common breath components and solvents. Each of the 35 inebriated participants gave an acceptable sample. Because of the metabolism of 2-propanol, the subjects exhaled high concentrations of acetone in addition to ethanol. Other volatile ingredients of technical ethanol products (methyl ethyl ketone, methyl isobutyl ketone, and 2-propanol) were also detected. The lower limits of quantification for the analyzed components ranged from 1.7 to 12 microg/L in simulated breath samples. The bias was +/-2% for ethanol and -11% for methanol. Within-day and between-day coefficients of variation were <1% for ethanol and <4% for methanol. The bias of ethanol and methanol analyses due to coexisting solvents ranged from -0.8 to +2.2% and from -5.6 to +2.9%, respectively. The FT-IR method proved suitable for use outside the laboratory and fulfilled the quality criteria for analysis of solvents in breath.     

A fatal case of pure ethanol ingestion

An adult male was found dead in a car with two empty bottles (500 ml x 2) labeled dehydrated ethanol (>99.5%, v/v). At autopsy, extensive pancreatic necrosis with severe hemorrhage was observed. High concentrations of ethanol were detected in blood (8.14 mg/ml), urine (8.12 mg/ml) and tissue specimens. The cause of death was determined to be an acute alcohol intoxication caused by ingesting approximately 1l dehydrated ethanol.     

A kinetic model describing the pharmacokinetics of ethyl glucuronide in humans

The glucuronide conjugation is a minor pathway of ethanol metabolism. The determination of ethyl glucuronide (EG) in serum and urine has gained importance in forensic and other legal decisions. To prospectively calculate the serum concentration of this non-oxidative ethanol metabolite, the computer program developed includes a parameter fitting routine. Multiple ethanol doses can be handled.The mathematical modeling was based on the following assumptions and simplifications, respectively. A single enzyme system is responsible for ethanol conjugation at one distinct site; the distribution of EG into the systemic circulation is delayed; the elimination of EG follows first-order kinetics.The concentration of EG was calculated using three kinetic parameters: a rate constant for the first-order formation of EG from serum ethanol, a transfer constant for an obstructed transfer of EG from the formation site (FS) into the central compartment (CC) and an exponential elimination constant.The program was applied to the data collected from 21 drinking experiments. The fitting algorithm optimized the three kinetic parameters, until the sum of concentration error squares of the data points was minimized. The means+/-standard deviation of the rate constant for the first-order formation of EG from serum ethanol was 0.0011+/-0.0006 h(-1), the transfer constant for an obstructed transfer of EG from the FS into the CC was 0.43+/-0.1996 h(-1) and the exponential elimination constant was 3.0+/-1.45 h(-1).Using the range of these parameters, it is now possible to calculate minimum and maximum serum concentrations of EG based on ethanol doses and drinking times. The comparison of calculated and measured concentrations can prove the plausibility of an alleged ethanol consumption. This can be crucial when the serum ethanol concentration (SEC) itself is not meaningful.     

Bite marks: physical properties of ring adhesion to skin-phase 1

Abstract: Unsupported excised skin may shrink by as much as 50% or more. In 1981, a method was developed for ring adhesion to skin with the goal of minimizing tissue distortion upon excision. Five modified versions of the technique bearing the author’s name followed (Dorion types I, II, III, IV, and V). The scientific literature reveals little supporting empirical evidence for the preferential use of one adhesive/suturing technique over another. This study compares the use of various bonding materials (Loctite Super Glue gel^®, Dermabond?, Vetbond?), cleaning agents (ethanol, dishwashing liquid, and shaving cream), and depilatory (Veet^®) on the effects of ring adhesion to skin. The conclusions indicate that surface wetness is the most influential factor affecting ring adhesion to skin, followed by the type of bonding material, its “freshness,” and by the cleaning agent used to prepare the skin. The use of a depilatory or shaving cream is to be avoided.     

Comparative analysis of gamma-hydroxybutyrate and gamma-hydroxyvalerate using GC/MS and HPLC

This paper describes two analytical techniques used to separate and quantify gamma-hydroxybutyrate (GHB) and gamma-hydroxyvalerate (GHV). The first technique was a N,O-bis(trimethylsilyl)triflouro-acetimide-trimethylchlorosilane derivatization, followed by gas chromatography/mass spectrometry analysis using an HP-5 capillary column at a rate of 1.0 mL/min with a run time of 9.25 min. This technique was found to be sensitive (LOD 1 pg on column) and gave a low average error (5%) in a beverage study. When supplemented by a surrogate spike, the method yielded 97% analyte recovery from beverages. The second technique was high-performance liquid chromatography/UV (HPLC/UV) using a C-18 column with a (20:80% v/v) methanol:dibasic phosphoric buffer (10 mM, pH 3) at a rate of 1.00 mL/min with a run time of 7.5 min. UV detection occurred at 254 nm. This method was found to be less sensitive (LOD 0.05 microg on column) for direct analysis of aqueous samples. To remove interferences seen in the beverage study, a liquid-liquid extraction before HPLC analysis was tested. However, a decreased sensitivity (LOD 100 microg on column) and irreproducible peak profiles resulted.     

A Simple Solubility Tests for the Discrimination of Acrylic and Modacrylic Fibers

In a crime scene investigation, single fibers play an important role as significant trace physical evidence. Acrylic fibers are frequently encountered in forensic analysis. Currently, acrylic and modacrylic are not discriminated clearly in Japan. Only results of FT‐IR, some of acrylics were difficult to separate clearly to acrylic and modacrylic fibers. Solubility test is primitive but convenient useful method, and Japan Industrial Standards (JIS) recommends FT‐IR and solubility test to distinguish acrylic and modacrylic fibers. But recommended JIS dissolving test using 100% N,N‐dimethylformamide (DMF) as a solvent, some acrylics could not be discriminated. In this report, we used DMF and ethanol (90:10, v/v) solvent. The JIS method could not discriminate 6 acrylics in 60 acrylics; hence, DMF and ethanol (90:10, v/v) solvent discriminated 59 of the 60 fibers (43 acrylic and 16 modacrylic fibers) clearly, but only one modacrylic fiber incorrectly identified as acrylic.     

慢性乙醇中毒小鼠脑神经细胞IP3R1表达的变化

目的研究慢性乙醇中毒引起小鼠脑神经细胞Ⅰ型1,4,5-三磷酸肌醇受体（IP3R1）表达的变化。方法 40只小鼠随机分为90d、180d组,各组再分为正常对照组、10%、20%、30%乙醇组,每组5只,乙醇组给予相应浓度乙醇饮用至相应时间;取各组小鼠脑组织,分别采用免疫组化和Western blot方法检测脑皮质神经细胞IP3R1表达的变化;SPSS 13.0软件对实验数据进行单因素方差分析。结果正常IP3R1免疫组化染色物分布于神经细胞胞浆内。90d组随乙醇浓度的增加,IP3R1免疫组化阳性细胞数和阳性细胞率逐步增加,组间比较,差异显著（P〈0.05）;180d组中10%、20%乙醇组阳性细胞数和阳性细胞率逐步增加,组间比较,差异显著（P〈0.05）,而30%乙醇组阳性细胞数和阳性细胞率反而减少,且低于90d组的相同浓度组（P〈0.05）。Western blot与免疫组化检测结果基本一致。结论慢性乙醇中毒可引起小鼠大脑皮质神经细胞IP3R1表达增加,而高浓度（30%）、长时间（180d）乙醇使IP3R1表达降低,可能与神经细胞变性、坏死、数目减少有关。