固相萃取-气相色谱法检测生物检材中斑蝥素

目的建立固相萃取-气相色谱法检测生物检材中斑蝥素的方法。方法采用HLB固相萃取柱提取,气相色谱-内标法检测。结果斑蝥素在0.1～200mg/L范围内呈良好的线性关系,相关系数为0.999以上;精密度（RSD）小于5%。对于添加血样,方法检出限为0.05μg/mL,加标回收率范围为93.03%～98.29%。结论该方法操作简便、快速、灵敏,提取回收率高,提取物含杂质较少,可用于实际案件中全血和尿样中斑蝥素的检测。     

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）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。     

全血中苯骈二氮杂类药物的胶束电动色谱法分析

目的建立用固相萃取胶束电动毛细管色谱法测定人体全血中苯骈二氮杂艹卓类药物的方法。方法全血以Oasis小柱提取,以克仑特罗为内标,采用未涂层毛细管(75μmID×50.2cm,有效分离长度为40cm),缓冲液为30mmol/LSDS→15mmol/L硼砂→15mmol/L磷酸盐(pH8.2)→18%甲醇。进样条件:压力进样0.5psi×10s,分离电压为25kV,柱温25℃,检测波长为230nm。结果本法分离效率高,9种苯骈二氮杂艹卓类药物的最低检测浓度为5～50ng/ml;血药浓度的线性范围为0.02～1.6μg/ml,日内、日间精密度<12%。结论本法简便、高效、可靠。     

保存犬尸体中自生醇的研究

目的建立组织中自生醇直接进样毛细管柱气相色谱检测方法；建立犬尸体中自生醇研究模型．观察犬尸体中自生醇的产生情况。方法犬经CO2处死，置于室温，分别于死后0、2、4、8、12、24、48、72、96、120h采集样品，样品匀浆后（体液除外）离心去上清，内标溶液1：2（体液为1：4）稀释，直接进样，气相色谱法检测，保留时间定性，内标法定量。结果甲醇、丙酮、乙醇、正丙醇、异丁醇、异丙醇、正丁醇、异戊醇的保留时间分别为（2．77±0．01）、（3．42±0．01）、（3．87±0．01）、（5．92±0．01）、（7．54±0．01）、（7．92±0．01）、（10．33±0．01）、（13．55±0．01）min；大部分组织如心血、下腔静脉血、尿、胆汁、肝、脾、肺和肾在犬死后12h可检出乙醇，肌肉、玻璃体液、和大脑分别在死后48、72、96h检出乙醇；乙醇和正丙醇的生成存在正相关。结论死亡犬体内会产生自生醇，尿中检出乙醇不能判定为生前饮酒，在涉及乙醇的法医学检案中。特别是腐败样品．应注意自生醇对乙醇定性和定量可能造成的影响，应采集不易腐败的组织如玻璃体液、肌肉或大脑，检测乙醇及自生醇含量，并观察与正丙醇的比例关系来进行综合判定。     

LC-MS/MS分析人全血中五氟利多

目的建立人体全血中五氟利多浓度的液相色谱-质谱联用法（LC-MS/MS）分析方法。方法全血中五氟利多和利培酮（内标）经正己烷液-液提取后,采用Capcell Pak C18色谱柱（250mm×2.0mm5,μm）进行分离,流动相为乙腈：20mmol/L乙酸胺和0.1%甲酸溶液（75∶25,V/V）,流速为0.2mL/min,然后以MS/MS电喷雾正电离的多反应监测扫描方式（MRM）测定。用于定量分析的离子为m/z 524→109（五氟利多）和m/z 411→191（内标）。结果五氟利多的最低检测限为0.2ng/mL,在0.4～400ng/mL浓度范围内线性良好（r=0.9994）,低、中、高浓度（1ng/mL、10ng/mL、100ng/mL）准确度分别为97%,108%和95%,日内和日间RSD均小于15%。结论该方法简便、快速、灵敏,适用于全血中五氟利多浓度的测定。     

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。     

超快速气相色谱电子鼻分析技术在汽油标号判定中的应用研究

目的采用电子鼻（超快速气相色谱仪）对汽油样品分析。方法用主成分分析法（PCA）对样品中的色谱峰进行数据处理并建立模型,对不同汽油标号（90#、93#、97#）进行归类和判定。气体顶空进样/快速气相色谱法主要条件：进样体积500μL;进样口温度250℃;进样时间5s;数据采集时间5min;热脱附温度280℃;程序温度40℃（30s）-1℃/s-280℃（30s）;FID温度280℃。结论利用超快速气相色谱和电子鼻指纹分析技术,可以用于未知汽油样本的定性和汽油标号判定。     

固相萃取-液相色谱-串联质谱法测定全血中多塞平

目的建立固相萃取-液相色谱-串联质谱（SPE-LC-MS/MS）分析全血中多塞平的方法。方法以阿米替林为内标,全血样品经固相萃取处理后,通过液相色谱-串联质谱技术进行检测（电喷雾离子源正离子方式,多反应监测模式）。监测离子对m/z多塞平为280→107、280→235、280→220,阿米替林为278→233。多塞平和阿米替林的保留时间分别为15.15min和16.94min。结果全血中多塞平在0.005～1.00μg/mL质量浓度范围内呈线性关系,线性方程为y=3.2047x＋0.0339,相关系数（r）=0.9996,检出限为0.001μg/mL;平均提取回收率为78.0%～82.9%,日内精密度〈2.55%,日间精密度〈5.90%。结论本方法快速简便、灵敏、重现性好,适用于全血中多塞平的检测。     

气相色谱-质谱法测定涉案奶粉中辛硫磷的含量

目的 建立基于气相色谱-质谱法（GC-MS）测定奶粉中辛硫磷含量的方法。方法 对待测样品进行乙酸乙酯萃取,利用Florisil固相萃取柱净化,淋洗液供GC-MS分析,设置适当的色谱质谱条件分析检测。结果 该方法在0.10～5.00 mg/L内具有良好的线性关系,辛硫磷在奶粉中的最低检出限为0.05 mg/L,加标回收实验结果表明,辛硫磷在奶粉中的平均回收率为98.2%～101%,相对标准偏差为2.1%～3.1%。案件检材样品在保留时间约8.377 min处出现与辛硫磷标准品相似色谱峰,且质谱定性离子[m/z 109（基峰）、m/z 135、m/z 298]与辛硫磷标准溶液一致,辛硫磷的含量为2.17 mg/kg。结论 该方法操作简单、灵敏度高、可行性强,可用于检测奶粉中的辛硫磷成分,为其他辛硫磷检测提供有益借鉴。     

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。     

血液中64种常见有机氯菊酯类农药的快速筛查

目的建立人体血浆中64种有机氯菊酯类农药多残留的气相色谱（GC）快速筛查分析方法。方法空白人体静脉抗凝血用乙腈沉淀蛋白,乙酸乙酯∶环己烷（v/v,3∶1）进行液液萃取净化,使用HP-5色谱柱,采用气相色谱进行定性、定量分析。对方法进行优化并进行方法学评价。结果 64种农药在0.001~0.1μg/mL范围内线性关系均良好,相关系数在0.990 1~0.999 9之间。检出限在0.001~0.15μg/mL范围内,方法定量限在0.001~0.5μg/mL之间,回收率总体于80%~110%之间,相对标准偏差小于15%,方法检出限总体于0.01μg/mL以下,日内精密度在1.5%~11.5%之间,日间精密度在2.9%~13.9%之间。结论本文建立的人体血浆的农药多残留快速筛查测定法,符合农药残留分析方法的要求,可在相关研究和实践中选用。     

Physiological variations in blood ethanol measurements during the post-absorptive state

Specimens of arterial plasma and venous whole blood were obtained at 3-10 min intervals during the post-peak phase of ethanol metabolism in healthy volunteers. The concentrations of ethanol in blood and plasma were determined by headspace gas chromatography. This method had a standard deviation of 0.28 mg/dl for whole blood and 0.26 mg/dl for plasma and the coefficients of variation were 0.43% and 0.79% respectively. The physiological variation from time-to-time, expressed as the residual standard deviation after fitting the ethanol concentration-time regression relationships, ranged from 0.43-3.7 mg/dl (0.65-16%). The time-to-time variations in concentrations of ethanol were maximum when there were problems in getting an unimpeded flow of blood through the indwelling catheters. The results do not support the existence of sporadic fluctuations or spiking in the blood alcohol concentration-time profile during the post-absorptive state. Instead, this study underscores the need to control carefully the method of sampling blood and in this way keep pre-analytical sources of variation to a minimum.     

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。     

Analysis of 2-hydroxyimipramine in an imipramine-related fatality

A fatality following ingestion of the tricyclic antidepressant imipramine (Novopramine), acetaminophen, and ethyl alcohol is described. Imipramine, desipramine, acetaminophen, and 2-hydroxyimipramine were quantitated by high performance liquid chromatography, and ethyl alcohol by gas liquid chromatography. Concentrations of imipramine, desipramine, 2-hydroxyimipramine, and acetaminophen were: in blood--9.0, 1.1, 3.9, and 11 mg/L; in urine--92, 14, and 42 mg/L (acetaminophen not quantitated in urine). Ethyl alcohol concentration in blood was less than 10 mg/dL and 105 mg/dL in the urine by headspace gas chromatography. These findings are compared to previous reports of imipramine-related fatalities. To our knowledge, this is the first fatality reported involving imipramine where analysis included quantitation of 2-hydroxyimipramine in blood and urine.     

血液乙醇检测内外标法比较研究

目的通过比较内标法和外标法对血液乙醇含量检测结果,探讨外标法在法医学实践中的应用价值。方法通过收集2005年10月~2006年12月间本中心符合检测要求的血液样品263例,每例分别采用内标法和外标法进行血液样品乙醇含量检测,比较其检测结果。结果外标法检测时间短(2.5min),用量0.5ml,而内标法检测时间长(6.5min),样品量1.0ml;外标法检测血乙醇平均浓度为89.30mg/100ml,内标法检测血乙醇平均浓度为92.37mg/100ml,P=0.001。结论外标法检测时间短(2.5min),用量少,节约检材,可作为大量待测血液样本的筛选检查手段。     

Computer-aided headspace gas chromatography applied to blood-alcohol analysis: importance of online process control

This paper describes the analysis of ethanol in blood specimens from suspect drunk drivers and the associated quality assurance procedures currently used in Sweden for legal purposes. Aliquots of whole blood from two separate Vacutainer tubes are diluted with 1-propanol as internal standard before analysis by headspace gas chromatography (HS-GC) with three different stationary phases: Carbopak B, Carbopak C, and 15% Carbowax 20 M. The actual HS-GC analysis, the integration of chromatographic peaks, the collection and processing of results, as well as the quality control tests involve the use of computer-aided techniques. The standard deviation of analysis(y) increased with concentration of ethanol in the blood specimen(x), and above 0.50 mg/g the regression equation was y = 0.0033 + 0.0153x. The prosecution blood-alcohol concentration (BAC) is the mean of three separate determinations made by different laboratory technicians working independently with different sets of equipment. A deduction is made from the mean analytical result to compensate for random and systematic errors inherent in the method. At BACs of 0.5 and 1.5 mg/g, which are the statutory limits in Sweden, the allowances currently made are 0.06 and 0.09 mg/g, respectively. Accordingly, the reduced prosecution BAC is less than the actual BAC with a statistical confidence of 99.9%.     

A fatality involving clomipramine

A fatality following ingestion of the tricyclic antidepressant clomipramine (Anafranil), alprazolam (Xanax), and ethyl alcohol is described. Clomipramine and N-desmethylclomipramine were quantitated by high performance liquid chromatography and alprazolam by gas liquid chromatography. Concentrations of clomipramine and N-desmethylclomipramine were: in blood--0.84 and 1.4 mg/L; in urine--0.56 and 0.62 mg/L. Alprazolam concentration in blood was 0.069 mg/L. Ethyl alcohol was measured by headspace gas chromatography and found to be 375, 385, and 435 mg/dL in blood, urine, and vitreous humor, respectively. These findings are compared to previous reports of clomipramine related fatalities and alprazolam toxicity combined with ethyl alcohol.     

A carpipramine related fatality

A fatality following ingestion of the tricyclic antidepressant carpipramine (Prazinil) and ethyl alcohol is described. Carpipramine was quantitated by high performance liquid chromatography. The concentration of carpipramine was 2.0 mg/L in blood and 0.44 mg/L in urine. Ethyl alcohol was measured by headspace gas chromatography and found to be 105 mg/dL in blood and 55 mg/dL in the urine. Quantitative analysis of stomach contents was positive for carpipramine by thin-layer chromatography. To our knowledge, this is the first reported fatality involving carpipramine.