HPLC／MS检测生物样品中的丁丙诺啡

目的建立了生物样品中丁丙诺啡的高效液相色谱-电喷雾串联质谱检测方法。方法样品经固相萃取提取净化、反相液相色谱分离后进行质谱检测，根据保留时间及特征离子进行定性分析，以母离子m／z468进行定量分析。结果在10-500ng／ml（ng／g）范围内峰面积与质量浓度的线性关系良好（r^2〉0．993）。在50、100、500ng／ml（ng／g）3个添加水平，尿、血、肝中丁丙诺啡的平均回收率为74％～94％，日内测定结果的相对标准偏差小于8％，日间测定结果的相对标准偏差小于10％。结论该方法简单、灵敏，特异性强，适用于生物样品中丁丙诺啡的分析检验。     

尿中氯喹定性定量分析方法的研究

建立了人尿中氯喹的定性定量分析方法,2ml尿样用2ml×2环己烷：乙酸乙酯（8：2）提取净化后,60℃水浴室气吹干,残留物定容溶解后,气相色谱分析,氯喹的保留时间为9．44min。方法最低检测限为200ng／ml,回收率为87．0％,RSD＝7．9％（n＝5）,在0～50μg／ml浓度范围内,有良好的线性关系：A＝1778．9＋13686C,r＝0．999。方法同时可用于血中氯喹的分析。附一例应用报告,测得尿中氯喹的含量为0．745mg／ml,血中氯喹的含量为3．68μg／ml。尿液中同时检出氯喹的N－去单已基代谢物。定性结果经质谱法验证。     

血中苯酚及甲酚的固相萃取-GC/MS分析

用固相萃取－GC／MS对人血中的酚和甲酚进行定性和定量分析。采用GDX403对分析物和邻氯酚（内标）进行固相萃取，并采集总离子流色谱。根据分析物在血中的浓度，通过总离子流色谱峰的质谱和保留时间或特征离子质量色谱峰保留时间进行定性分析。实验采用特征离子质量色谱进行定量分析，线性范围0．02～10μg／ml。本方法检测限为10ng／ml，CV％为2.11～4.20％，分析物和内标的萃取率为68．6～89．5％，血中添加测定回收率为97．8～104％。本法测定健康人血中苯酚含量为2．2±0．4μg／ml．     

HPLC法测定百草枯急性中毒大鼠的体内分布

目的 应用高效液相色谱法对口服百草枯急性中毒大鼠体内分布进行测定。方法以200mg／kg剂量百草枯给予Wister大鼠灌胃,4h后脱臼处死,解剖取脑、心、肝、脾、肺、肾、胃、盲肠、肌肉等组织,应用固相萃取法提取,液相色谱法测定各器官组织中百草枯含量。结果各组织经检验,均检出百草枯;组织间百草枯含量（μg／g）相差明显,其中最高为胃（231．47±129．10）,其次为盲肠（87．08±39．86）、肺（22．73±10．20）,最低为心（2．01±0．36）。结论百草枯口服给药后组织分布较为广泛,除胃、肠外各脏器中以肺浓度最高。     

顶空固相微萃取与气质联用快速检测尿液中氯胺酮及去甲基氯胺酮

目的建立利用顶空固相微萃取（HS／SPME）结合气相色谱／质谱联用技术（GC／MS）快速检测吸毒人员尿液中氯胺酮（KT）及其主要代谢物去甲基氯胺酮（NK）的方法。方法样品瓶中加入尿样、6mol／L氢氧化钠溶液、固体氯化钠、SKF525A（内标），85℃下加热搅拌，用100μm聚二甲基硅氧烷（PDMS）萃取头顶空萃取10min，GC／MS（EI-SIM）检测。结果尿液中NK和KT浓度在0．1～2．0μg／ml范围内呈现线性关系，相关系数分别为（r^2）0．9991和0．9945，检测限（D／N=3）分别为0．87ng／ml和2．76ng／ml，定量限（S／N=10）分别为2．90ng／ml和18．52ng／ml。1ml尿液加标600ng，NK回收率在85．5％～110．1％，RSD〈13．2％（n=6）；KT回收率在77．5％～109．6％，RSD〈511．99％（n=6）。结论建立的方法简单、快速、灵敏、准确，适合尿液等生物检材中NK及KT的快速定性定量分析。     

GC法检测血液和尿液中甲基苯丙胺和咖啡因

目的建立同时测定血、尿中甲基苯丙胺和咖啡因含量的方法。方法应用GC／NPD技术,以4-苯基丁胺为内标,直接碱化,用氯仿提取,三氟乙酸酐衍生化,8CB熔融石英毛细管柱（30m×0．25mm×0．25μm）分析。结果生物样品中甲基苯丙胺与咖啡因在0．012—7．5μg/mL浓度范围内线性关系良好,检测限（S／N=3）依次为1．2ng／mL,0．6ng／mL（血）;1．6ng／mL,0．8ng／mL（尿）。苯丙胺在0．017—10．0μg／mL浓度范围内线性关系良好,检测限为1．6mg／mL（血）,3．2ng／mL（尿）。所有样本回收率均大于85％。结论本方法准确、灵敏,适用于血、尿中甲基苯丙胺及其代谢物苯丙胺的三氟乙酸酐衍生化物和咖啡因的同时检测,为判定滥用毒品种类、追查毒品来源以及研究生物体内甲基苯丙胺和咖啡因的交互影响提供了检测手段。     

气相色谱法同时测定血清中甲醇、乙醇、正丙醇

目的建立气相色谱同时测定血清中甲醇、乙醇、正丙醇含量的方法。方法改变气相色谱条件,以异戊醇为内标,采用气相色谱一氢火焰离子化检测器对血清直接进行检测。并通过待测组分与内标物的响应值比进行定量。结果GC／FID法检测血清中的甲醇、乙醇、正丙醇含量,得到了良好的线性关系。乙醇浓度从1～100mg／100ml。的线性关系式为Y=0．4145X＋0．0232（R2=0．9974）、浓度从100～1000mg／100mL的线性关系式为Y=0．4511X＋0．0746（R2=0．9911）,甲醇浓度从l-200mg／100mL的线性关系式为Y=0．2778X＋0．0493（R2=0．9983）。结论该方法操作简便快速,重现性好,通过检测正丙醇还可以推断腐败血样自身产生的乙醇量,是一种较为理想的血醇检测方法。     

应用ELISA测定成人皮肤切创纤维连接蛋白

应用双抗体夹心酶联免疫吸附剂测定法（ELISA），定量研究了12例成人腹部2小时以内手术切创皮肤可检测的Fn。实验批内变异系数＜5％，批间变异系数＜10％，检测Fn浓度范围3．91～1000ng／ml。结果：成人腹部每克皮肤可检测Fn含量为7．5920±1．7364μg（M±SD）；随着损伤时间延长，不同时间段创伤局部皮肤Fn的含量逐渐升高；各不同时间段与损伤即刻皮肤Fn含量的差值和损伤时间之间存在直线相关（r=0．9843）。经方差分析处理，发现创伤局部皮肤Fn含量在损伤经历30分钟后，有显著增加。本此结果可为推断切创形成的时间提供参考数据。     

尿中MDMA及其代谢物的GC和GC／MS分析

考察MDMA在人体内的代谢以及建立尿中MDMA和体内主要代谢物MDA的分析方法。尿样水解后经液-液提取处理,用GC／MS（EI、PCI）和GC／FID法分析。人摄入MDMA后尿中MDA和原体MDMA比约为0．10～0．14。GC／MS／SIM和GC／FID法的最低检出限为2ng／ml和50ng／ml,回收率大于85％,变异系数小于10％。该法简便快速、灵敏度高、结果可靠,可用于MDMA滥用者的尿样鉴定。MDA／MDMA浓度比可作为评判毒分结果的参考指标。     

UPLC—MS／MS法测定人血中雪上一枝蒿甲素

目的建立超高效液相色谱-串联质谱（UPLC—MS／MS）法测定人血中雪上一枝蒿甲素含量的方法。方法样品经乙酸乙酯提取后,Ci8柱分离,以0．1％甲酸乙腈-0．1％甲酸水为流动相梯度洗脱,正离子-多反应离子监测模式（ESI＋-MRM）测定雪上一枝蒿甲素,定性定量离子对分别为344．3／58．0、344．3／91．0。结果雪上一枝蒿甲素在3．5～850ug／L-1。范围内与峰面积呈现良好的线性关系（r=-0．9968）,检测限为0．1Iμg／L-1,日内、日间精密度均〈10％,低、中、高三个浓度下准确度（n=5）为97．2％-115．2％,回收率（n=5）为86．6％~89．4％。结论该方法操作简便,结果准确,可作为测定人血中雪上一枝蒿甲素含量的方法。     

The relationship between alcohol elimination rate and increasing blood alcohol concentration--calculated from two consecutive blood specimens

In the period 1991-2005, a blood-alcohol concentration (BAC) analysis was carried out at the Institute of forensic medicine in Novi Sad including 2023 two consecutive blood specimens using the Headspace Gas Chromatography method. Cases with no alcohol concentration values, as well as cases where blood samples were taken within 1 h after the criminal act, were not taken into consideration. Following this rule, 1198 cases were considered in this study and all samples were grouped in 29 ranges of BAC1 of delta(BAC) = 0.1 g/kg, starting from 0.1-0.19 g/kg to 2.9-2.99 g/kg of absolute alcohol. Gathered results and elimination curve differ from the zero-order model of elimination proposed by Widmark and point to an elimination process similar to a well-known Michaelis-Menten elimination kinetics model and its variants. Results reported in this study show dependence of alcohol elimination rate (beta-slope) and BAC value. The analysis of beta60-slope versus BAC shows that a correlation between beta60 (y) and BAC (x) has a logarithmic trend line. The value of alcohol elimination rate shows a slight increment with increase of BAC alcohol, with the mean value of beta60 = 0.221 +/- 0.075 g/kg. Differences in values of beta60 among consecutive intervals of delta(BAC) = 0.1 g/kg are not significant (p>0.05). When obtained samples were grouped into ranges of 0.5 g/kg each in these intervals beta60 had the following values by range: 0.1-0.49 g/kg = 0.139 g/kg +/- 0.035; 0.5-0.99 g/kg = 0.184 g/kg +/- 0.043; 1-1.49 g/kg = 0.213 g/kg +/- 0.052; 1.5-1.99 g/kg = 0.239 g/kg +/- 0.058; 2-2.49 g/kg = 0.265 g/kg +/- 0.073; 2.5-2.99 g/kg = 0.306 g/kg +/- 0.096. Differences in values of beta slope among consecutive intervals of delta(BAC) = 0.5 g/kg are significant (p<0.01). The elimination curve in the BAC interval 0.5-2.5 g/kg has a linear trend, while beta-slope (y)/BAC (x) correlation is given as beta60 = 0.15 g/kg + (0.05 g/kg x BAC). Retrograde calculation of the blood alcohol concentration in tempore criminis (BAC(tc)) based on the determined alcohol concentration in the blood specimen (BAC(t)) shows a statistically significant difference between BAC(tc) calculated using a standard zero-order model versus corrected methodology. The higher the BAC(t) and the longer the calculation time, the greater and statistically more significant (p<0.01) is the difference between the calculated values of BAC(tc).     

The accuracy of blood alcohol analysis using headspace gas chromatography when performed on clotted samples

Subjects consumed alcoholic beverages and attained blood ethyl alcohol concentrations ranging from 0.02 to 0.15 g/dL. Sets of blood samples were drawn from these subjects, including some samples that were allowed to clot and some in which anticoagulent was added. A quantitative analysis for ethyl alcohol was performed on these samples using headspace gas chromatography. The mean deviation of the concentration of ethyl alcohol in the clotted samples from the ethyl alcohol concentration in the corresponding control samples was 0.001 g/dL. The 99% confidence interval for this mean was +/- 0.0005 g/dL.     

腐败血液中自生醇现象及法医学应用研究

目的 检测分析腐败血液中乙醇、甲醇等物质的生成过程,为正确判断案发时人血液中醇类物质的实际浓度提供实验依据.方法 以正常健康人血液制作腐败样本,分别模拟人死亡后正常人血液和糖尿病人高糖血液的腐败过程,借助顶空气相色谱仪测定两种血液腐败后醇/醛类物质的生成情况并对比含量差异.结果 相同实验条件下,高糖血液较正常健康血液更...     

Abnormally high alcohol concentration in the heart blood

A 46-year-old male alcoholic whose whereabouts had been unknown for about a month was found dead at the foot of a cliff 31 m deep. Fractures of the mandible, thorax and left patella were found at autopsy, but fatal injury to the brain or other organs was not observed. The alcohol distribution was 7.44 mg/g in the heart blood, 13.91 mg/g in the left thoracic cavity fluid and 1.88 mg/g in the urine. The high ethanol concentration in the heart blood was assumed to be mainly due to the diffusion of ethanol from the contents of the stomach and postmortem production of ethanol. It was decided that the cause of death was not acute alcohol intoxication but respiratory failure caused by fractures of the thorax.     

ALDH2基因多态性与乙醇代谢及外周乙醛积蓄程度的关系

目的了解不同乙醛脱氢酶2（acetaldehydedehydrogenase2,ALDH2）基因型人群饮酒后,其乙醇药代动力学和外周乙醛积蓄程度。方法收集无血缘关系的志愿者14名,采集静脉血液并且通过聚合酶链反应限制性片段长度多态性技术提取DNA并检测ALDH2基因型,按一定剂量饮酒后,以顶空气相色谱法于不同时间点同时测定血中乙醇及乙醛的含量并计算药代动力学参数。结果根据电泳结果,野生组为5名野生纯合型ALDH2＊1／＊1个体．突变组为9名突变杂合型ALDH2＊1／＊2个体,血中乙醇和乙醛分别在0～1570．7μg/mL和0～5．1772μg／mL范围内线性关系良好。突变组乙醇及乙醛药时曲线下面积（AUC）以及乙醇的末端消除半衰期（tl／2Z）均大于野生组,乙醇的经生物利用度校正的表观消除率（CL／F）小于野生组（P〈0．05）。结论饮酒后,ALDH2＊I／＊2突变组受酶活性抑制影响,血中乙醇和乙醛代谢减慢,造成外周乙醛的蓄积,从而进一步强化其在体内的作用。     

Determination of mouth alcohol using the Dräger Evidential Portable Alcohol System

Drivers suspected of alcohol intoxication are observed for a period of 15 min prior to quantitative breath alcohol testing. This is to preclude the interference of alcohol-based substances such as cough medicine, mouthwash, and breath spray just prior to actual evidential testing. To determine whether a 15 min observation period was necessary when performing evidential breath tests in the field, a mouth alcohol experiment was performed using the Dräger Evidential Portable Alcohol System (EPAS). Five types of alcohol beverages and the effects of expectorating versus swallowing were tested on twenty-five volunteer subjects. Serial measurements of breath and blood alcohol levels were performed at fixed time intervals. All alcohol beverage types gave two sequential measurements within 0.02 g/210 L of each other before 15 min had passed. Fifteen minutes was necessary to ensure there was no residual mouth alcohol. If the 15 min waiting period was not observed, the safety feature of the EPAS requiring two sequential measurements 2 min apart within 0.02 g/210 L would not ensure against mouth alcohol interference.     

Alcohol metabolism of local Chinese in Hong Kong: a statistical determination on the effects of various physiological factors

A study was designed to examine the elimination rate of alcohol from the body of the local Chinese after consumption of different types of alcoholic drinks. The breath alcohol of 184 healthy volunteers was determined and converted into blood alcohol levels after they finished drinking. Information on the type and volume of alcoholic drinks consumed, age group, sex, drinking habit, and drinking on empty stomach or with/after meal was recorded for each participant. The results show that the elimination rate of an individual can be explained in terms of physiological variables including sex and drinking habit. The determined elimination rates allow forensic toxicologists to back calculate the blood alcohol concentration (BAC) of the drivers at the time of accident in drunk driving cases. The elimination rates of blood alcohol at 95% prediction intervals for male and female are in the range of 9.5-23.8 mg/100 ml/h and 11.1-37.1 mg/100 ml/h, respectively.     

Effects of Homeopathic Mother Tinctures on Breath Alcohol Testing

In some countries, it is illegal to drive with any detectable amount of alcohol in blood; in others, the legal limit is 0.5 g/L or lower. Recently, some defendants charged with driving under the influence of alcohol and have claimed that positive breath alcohol test results were due to the ingestion of homeopathic mother tinctures. These preparations are obtained by maceration, digestion, infusion, or decoction of herbal material in hydroalcoholic solvent. A series of tests were conducted to evaluate the alcoholic content of three homeopathic mother tinctures and their ability to produce inaccurate breath alcohol results. Nine of 30 subjects gave positive results (0.11–0.82 g/L) when tests were taken within 1 min after drinking mother tincture. All tests taken at least 15 min after the mother tincture consumption and resulted in alcohol-free readings. An observation period of 15–20 min prior to breath alcohol testing eliminates the possibility of false-positive results.     

Acute lethal alcohol intoxication (author's transl)]

In 14,744 autopsy cases from an 18-year period 92 cases (of which 7 were ruled out because of decomposition were observed in which death was supposed to be due to direct acute alcoholic intoxication. In the police reports 81 persons were designated as chronic alcoholics or abusers of spirits. The blood alcohol level ranged between 2.04 and 4.92 o/oo. The cases studied were divided into two groups, one with low and the other with high lethal alcohol level. Fatty liver and cirrhosis were found with identical frequency in the two groups, whereas cardiac hypertrophy of obscure origin occurred markedly more often in the group with low lethal blood alcohol level. On the basis the possible mechanism of death in the cases with cardiac hypertrophy is discussed. Finally, the relation between the blood and urine alcohol concentrations observed in 72 cases is discussed. On the assumption that the water phase of the blood was 75 per cent of the total blood, death occurred in the persons without cardiac hypertrophy with fairly identical frequency either in the phase of absorption or the phase of elimination, whereas in the persons with cardiac hypertrophy death most often occurred in the phase of absorption. These statements should, however, be taken with some reservation, partly because the water phase of the blood may vary considerably post mortem (60-90 per cent) and partly because the urine alcohol concentration depends on serval variable factors.     

Excretion of alcohol in urine and diuresis in healthy men in relation to their age, the dose administered and the time after drinking

Healthy male volunteers drank neat whisky in amounts corresponding to 0.51, 0.68, or 0.85 g ethanol/kg body weight in 15-25 min after an overnight (10 h) fast. Urine was collected immediately before drinking and then at 60 min intervals for 7-8 h after intake. The volumes of urine voided were measured and the concentrations of alcohol (UAC) were determined by an enzymatic method. Ethanol-induced diuresis showed large inter-subject variations. The flow of urine was maximum between 60 and 120 min post-drinking when the median rates of production were 117 ml/h (range 55-335), 113 ml/h (range 41-453) and 373 ml/h (range 215-485) for 0.51, 0.68, and 0.85 g ethanol/kg respectively. The output of urine returned to normal (30-60 ml/h) after the peak UAC had passed despite an elevated blood alcohol concentration (BAC). The average amount of alcohol excreted in urine was 0.29 g (S.D. 0.119), 0.44 g (S.D. 0.246), and 1.00 g (S.D. 0.427) after the consumption of 0.51, 0.68 and 0.85 g ethanol/kg respectively. Neither peak diuresis nor the amount of alcohol excreted depended on a subject's age between 20 and 60 years. This work shows that after drinking a moderate dose of alcohol, only 0.7-1.5% of the amount consumed is excreted unchanged in urine. Ethanol-induced diuresis is most pronounced for the first 1-2 h after drinking (rising BAC). The production of urine returns to normal during the post-absorptive state.