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。     

血液样品中乙醇稳定性的实验研究

目的考察在不同存放条件下含乙醇的血液样品中乙醇浓度的变化情况。方法采用顶空-气相色谱法,以异丙醇为内标,对存放条件不同的血液样品中乙醇进行检测。结果冷冻(-10℃)条件存放1至30天,血液样品中乙醇含量无显著变化;冷藏(4℃)条件存放1至30天,血液样品中乙醇含量变化不显著;室温(28℃~33℃)条件存放1至30天,血液样品中乙醇含量显著改变。结论含有乙醇的血液样品,在冷冻、冷藏条件下可较稳定的存放30天;在室温条件下存放30天血液样品中乙醇浓度发生显著变化,不可在此条件下存放。     

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。     

高效液相色谱法测定盐酸曲马多血药浓度

目的 建立测定人血浆中盐酸曲马多浓度的HPLC-UV法。方法 血浆样品经碱化后,用二氯甲烷提取。采用依利特C18色谱柱(5μm),流动相为乙腈-磷酸盐缓冲液(74:26,pH6.5),检测波长为220um。结果 盐酸曲马多浓度在10～800ng/ml范围内与曲马多/内标物峰高比呈良好线性关系,r=0.9984,平均回收率为93.48％,最低定量检测浓度为10ng/ml;日内及日间RSD分别为3.81％～5.44％和3.95％～4.41％。结论HPLC-UV法用于血浆中盐酸曲马多浓度的检测,符合司法毒物分析及临床药血浓度测定的要求。     

直接进样气相色谱法测定全血中乙醇的含量

目的建立一种直接进样气相色谱法检测全血中的乙醇。方法全血经硫酸铝钾沉淀蛋白,加入内标异丙醇后,用直接进样气相色谱法进行检测,FID为检测器,用保留时间定性,内标标准曲线法定量。结果该方法线性范围为0.2-1.4mg/m L,相关系数R=0.999 3,总分析时间不超过5min,最低检测限为0.01mg/m L,相对标准偏差（RSD）〈5%,平均回收率为92.3%;所建立的方法与顶空气相色谱（HS-GC）法比较相对偏差（RD）〈10%。结论该方法可用于全血中乙醇的检测。     

人血中乙醇含量的分光光度法检测

本文介绍用分光光度法检测乙醇在0～600μl/100ml人血中浓度范围内的含量测定,具有简便、快速、检材用量少的特点,已成功地应用于多起案件的检验。     

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。     

血液中乙醇保存稳定性研究

目的确定血液中乙醇最佳保存条件,探讨影响血液中乙醇含量稳定性的主要因素。方法对血液保存的温度(-20、4、20℃)、防腐剂(NaF、无防腐剂、Na2O2)、储存容器中空气所占比例(0%、25%、50%)和血醇质量浓度(0.2、0.8、2.0mg/mL)四个因素采用正交试验L9(34)方法分组,样本采用顶空气相色谱法进行测定,测定结果采用方差分析进行讨论。结果在20℃保存且不加入防腐剂的两组样本中血醇浓度变化明显,其余变化不明显。结论血液样本在4℃、储存容器中空气比例为50%和加防腐剂(NaF)的条件下保存,稳定性最佳;四个影响因素中温度为影响血液中乙醇含量稳定性的主要因素。     

腐败血液中乙醇的顶空气相色谱分析

目的分析血液腐败后产生的乙醇及其他物质并探讨腐败血液中乙醇的检测及计算方法。方法以正常人空白血液制作腐败血样,采用1,4-二氧六环为内标物,通过顶空气相色谱进行定性及定量分析。结果血中乙醇在0.0625～1mg/mL范围内线性关系良好（r^2=0.9996）,各质量浓度组的变异系数（CV%）〈2%,血中乙醇的最低检出限为1μg/mL（S/N≥3）。腐败血样所产生乙醇与正丙醇的比例大致为25：1。结论检验方法简便、准确。为法医毒化检验相关工作提供了依据。     

HS-GC内标曲线法测定血中乙醇含量的不确定度评估

目的建立自动顶空-气相色谱(HS-GC)内标曲线法测定血中乙醇含量的不确定评估方法。方法从分析测定程序着手,依据不确定度评定的指导性文件,分析不确定度来源,量化不确定度分量,计算检测结果的合成标准不确定度和扩展不确定度。结果各相对不确定度来自于检材重复性检测为3.4%,乙醇标准溶液为0.71%,检材为0.61%,叔丁醇内标溶液为0.41%,标准曲线为1.1%,气相色谱仪为1.3%,血液中乙醇的相对扩展不确定度为3.9%。结论血液中乙醇含量的不确定度主要来源于检材重复性检测、气相色谱仪、乙醇标准曲线。     

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.     

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.     

Evaluation of breath alcohol instruments II. In vivo experiments with Alcolmeter Pocket Model

The precision and accuracy of an Alcolmeter Pocket Model breath alcohol instrument have been investigated in experiments with human subjects under controlled conditions. The instrument response was zero in all tests with breath samples from alcohol-free subjects. The standard deviations of ethanol determinations in breath were ±0.0722 mg/ml during ethanol absorption and ±0.0416 mg/ml during ethanol elimination. The standard deviation during the elimination phase increased with ethanol concentration in the sample, being ±0.0416 mg/ml on average at a mean concentration of 0.420 mg/ml, corresponding to a coefficient of variation of 9.9%.The blood alcohol estimates using the Alcolmeter were somewhat too high during active absorption of ethanol, and too low during elimination, when a constant blood-breath alcohol ratio of 2100:1 was used to calibrate the instrument. During the elimination phase of ethanol kinetics and at a mean blood alcohol concentration of 0.50 mg/ml, the mean Alcolmeter result was 0.456 ± 0.169 mg/ml with 95% confidence, i.e. varying between 0.287 and 0.625 mg/ml 95 times out of 100 tests at this critical blood alcohol level.     

A rapid method for blood alcohol determination by headspace analysis using an electrochemical detector.

A method for the determination of blood alcohol concentration by headspace analysis using an electrochemical detector is described. A determination can be made within 2 min, and only 0.1 ml of blood is required for each analysis. The detector response was linearly related to ethanol concentrations up to 3.0 mg/ml. The standard deviation of a single determination was +/- 0.014 mg/ml. The accuracy of the method based on comparison with an enzymatic (alcohol dehydrogenase) technique was high, the mean recovery being 102.2% of the attributed concentration. The ease of the operation and fast analysis time make the method ideal for serial determinations, for example during mass screening of biological samples for ethyl alcohol in forensic and toxicology laboratories.     

An analytical method for the rapid screening of organophosphate pesticides in human biological samples and foodstuffs

Gas chromatography with nitrogen/phosphorus sensitive detection (GC/PND) and electron impact mass spectrometry (GC/MS) with selected ion monitoring provides a simple, rapid and sensitive method for the determination of organophosphate pesticides (OPs). A selective single-step extraction of 23 different OPs in urine, blood, serum and food samples (baby food, soft drinks and instant soups suspected of contamination from a blackmailing scare) is described. The OPs were extracted with 1ml toluene (with and without addition of mevinphos as internal standard), using a 0.7ml aliquot of urine, blood or serum sample. Food samples (0.2g) were homogenised with water (0.5ml) before extraction. An amount of 1microl of the toluene phase (extraction supernatant) was analysed directly by GC/PND and GC/MS.The method was validated using spiked human serum. The OPs were mixed with serum containing 10mg/ml disodium ethane diamine tetraacetic acid disodium salt (EDTA disodium salt) and stored up to 10 days at 4 and -20 degrees C, respectively. The recovery rates of OPs in freshly spiked human plasma ranged between 50% (dimethoate) and 133% (dialifos). OPs in plasma proved to be stable at -20 degrees C. Their levels decreased only slightly after storage at 4 degrees C.     

体液中氟乙酰胺SPE-GC/MS检测

目的　利用GC/MS与固相萃取 (SPE)技术相结合 ,开发血和尿样中氟乙酰胺鼠药的GC/MS定量分析新方法 ,并用于实际案例检测。方法　选择乙酰胺为内标 ,通过比较不同固相柱的萃取效率和不同条件对回收率的影响 ,优化用于血和尿样中氟乙酰胺萃取的固相柱和提取条件 ,利用氟乙酰胺与乙酰胺质谱图的分子离子峰面积之比与氟乙酰胺浓度的定量关系 ,建立血和尿样中氟乙酰胺鼠药的GC/MS定量分析新方法。结果　用硅胶柱萃取 ,峰面积之比与氟乙酰胺浓度在 5 0～ 90 μg/ml范围呈线性关系 ,检测限为 1 0 μg/ml。血样中氟乙酰胺检测的平均回收率达 91 6% ,标准偏差小于 7 3 %。结论　此法对实际样品的测定证明可满足氟乙酰胺鼠药中毒的定性定量要求。     

固相微萃取-气相色谱质谱法测定血浆中的氯氮平浓度

目的建立固相微萃取-气相色谱质谱法测定人血浆中氯氮平浓度的方法。方法以固相微萃取法提取血浆中的氯氮平,萃取头为100μm聚二甲基硅氧烷,洛沙平作内标,用气相色谱质谱选择离子法进行检测。结果本文建立的方法在5~2000 ng/ml浓度范围内呈线性关系,检测限为0.1 ng/ml(信噪比>3),低、中、高浓度(100、500、1000 ng/ml)平均相对回收率分别为98.6%、94.6%和94.6%,日内、日间RSD分别小于7.4%和7.1%。结论本文建立的固相微萃取-气相色谱质谱法灵敏度高、准确度好、操作简便,适用于氯氮平急性中毒案件的检测。     

生物组织检材内异烟肼的薄层色谱扫描检测研究──附1例异烟肼中毒死亡者体内分布报告

改进血清中异烟肼的提取方法，建立了生物组织检材内异胭肼的提取和薄层色谱扫描检测方法，线性范围为2～32ug／ml或g，检出限为0．5ug／ml或g。l例异烟擀中毒死亡者体内异烟肼分布：肾31．6mg／100g、肝26．6mg／100g、脾22．1mg／100g、心21．3mg／100g、胃16．6mg／100g、脑15．5mg／100m、肺12．6mm／100g、小脑11．7mm／100g和10.5mm／100ml。