三甲基硫赶磷酸酯在甲胺磷农药中毒检验中的作用

目的探讨三甲基硫赶磷酸酯在甲胺磷农药中毒检验中的作用。方法利用气-质联用仪器(GC-MS)分析了甲胺磷中毒者的检材(血,胃内容物)。结果检出了O,O,S三甲基硫赶磷酸酯,却未检出甲胺磷。结论研究了这一现象的原因和确定了O,O,S三甲基硫赶磷酸酯(O,O,S-TMTP)可作为甲胺磷中毒的佐证物。     

有机磷农药薄层分析选用显色方法应注意的问题

本文介绍作者对薄层分析中三种不同显色法的显色效果与有机磷农药化学性质关系的一些体会。一、硫代磷酸酯类显色方法硫代磷酸酯类显色剂（即：氯化钯法、二氯配氯亚铵－溴法等）是有机磷农药薄层分析中最常用的显色方法。其显色原理是通过试剂对农药成为中的硫代磷酸酯的化学反应而显色。然而某些有机磷农药可在空气中氧化或在体内某些酶的作用氧化下，硫代磷酸酯中的硫将被氧取代，此时，采用检验硫代磷酸酯的显色方法，就不能检出。应当再选择乙醇－氢氧化钠显色确定有否硫代磷酯。二、对硝基酚显色法本法系对某些有机磷农药的特有官能团…     

用串联质谱法提高毒鼠强的检测灵敏度

目的建立一种能避免生物样品中杂质的干扰,提高毒鼠强检测灵敏度的方法。方法应用串联质谱法,对生物样品中的毒鼠强进行检验研究。结果在样品无需净化的情况下,以m/z240为母离子,当激活电压在0.8V左右时,毒鼠强二次电离的离子碎片适中,质谱谱图清晰;此时进样量为1.0ng的毒鼠强,其信噪比(s/n)为87,经与全扫描质谱法进行比较灵敏度大为提高。结论该方法能有效提高毒鼠强检测灵敏度,适用于同类案件检验。     

畜癞灵的薄层色谱法检验

畜癞灵是一种高效、低毒、杀菌范围广的体外杀虫剂,剂型含量16%乳油,畜癞灵主要用于杀灭猪、牛、羊、马、骆驼的疥螨、蜱类、虱类、蛋类、蝇类及虻类等体外寄生虫,其在内蒙古农牧区被广泛使用。笔者遇到两例使用此药中毒的案例,并成功对畜癞灵作了薄层色谱检验,效果很好,介绍如下。畜癞灵剂型为黄色乳油,室温于水中不溶,易溶于乙醚、二氯甲烷、乙醇,在中性条件下易提取。化学名称:O,O—二乙基—O—(3—氯—4—甲基香豆素—7—基)硫代磷酸酯,化学结构如图1。分子式:C14H16CLO5PS。分子量:362.76。图1畜癞灵的化学结构1实验方法1.1试剂和…     

新精神活性物质4F-MDMB-BUTINACA在斑马鱼体内的代谢

目的通过建立斑马鱼模型研究合成大麻素2-[1-(4-氟丁基)-1H-吲唑-3-甲酰氨基]-3,3-二甲基丁酸甲酯(4F-MDMB-BUTINACA)的体内代谢转化途径。方法将6条成年斑马鱼随机分为空白对照组和实验组,每组3条。实验组斑马鱼在4F-MDMB-BUTINACA(1μg/m L)药液中暴露染毒24 h后转移到清水中清洗3次,进行样品前处理,待仪器分析。空白对照组斑马鱼不暴露于4F-MDMB-BUTINACA。采用液相色谱-高分辨质谱技术结合Mass Frontier软件对4F-MDMB-BUTINACA及其代谢产物进行质谱解析和结构分析。结果斑马鱼体内共检测到4F-MDMB-BUTINACA的26个代谢产物,包括18个Ⅰ相代谢产物以及8个Ⅱ相代谢产物。4F-MDMB-BUTINACA在斑马鱼体内的Ⅰ相代谢途径主要包括酯水解、脱烷基化、氧化脱氟和羟基化,葡萄糖醛酸结合反应是主要的Ⅱ相代谢转化途径。结论酯水解代谢产物Md24和酯水解脱氢代谢产物Md25被推荐为4F-MDMB-BUTINACA滥用的良好生物标志物。     

亚甲基双氧甲基苯丙胺中毒检验方法的研究

详细讨论了亚甲基双氧甲基苯丙胺中毒后生物体内的提取、净化和检验方法,得出了生物体内亚甲基双氧甲基苯丙胺的提取最佳条件,净化方法和GC/FID定量分析方法,为类似毒品中毒的体内定性定量检验提供了参考.     

离子色谱法分析生物检材中的氯化琥珀胆碱

目的建立离子色谱法检验氯化琥珀胆碱分析方法。方法运用离子交换色谱使离子在分析柱中达到分离,采用电导检测器检测。结果实验的生物检材中准确检出琥珀胆碱及其它离子（Na^＋、NH4^＋、K^＋、Mg^2＋和Ca^2＋等离子）。结论该方法简便快捷,结果准确,可用于案件检验。     

GC/MS法联合分析生物检材中的尼美舒利、二氧丙嗪

目的建立生物检材中尼美舒利、二氧丙嗪的GC/MS检验方法。方法采用浸取法提取,GC/MS定性检验,内标法选择离子检测（SIM）模式定量检验。结果最低回收率为69%,尼美舒利的线性相关系数为0.998,克咳敏的线性相关系数为0.9973。结论该方法操作简便快速,提取率高,可用于实际案件中尼美舒利、二氧丙嗪的检验。     

用分时选择离子质谱法一次检测多种药物

目的建立一种能避免生物样品中杂质的干扰,一次排查多种药、毒物,准确、灵敏度高的检验方法。方法应用分时选择离子质谱法,对常见毒物进行检验研究。结果在样品经简单净化处理的情况下,以分时选择离子质谱法检测,一次检测多个毒物(最多32个),定性、定量准确,灵敏度50～100ng/ml,经与全扫描质谱法进行比较,灵敏度提高2～3个数量级。结论该方法能有效提高排查毒物检测灵敏度,适用于常见毒物的排查检验。     

超高效液相色谱-质谱法测定人全血中甲胺磷、乙酰甲胺磷含量

目的应用超高效液相色谱-质谱法(UPLC-MS/MS)对人全血中甲胺磷、乙酰甲胺磷进行定量测定。方法采用去离子水直接稀释人全血,提取血中的甲胺磷及乙酰甲胺磷,以甲醇-水(含0.1%甲酸)为流动相梯度洗脱,正离子化多反应监测(MRM)模式测定。结果甲胺磷、乙酰甲胺磷的回收率均高于87%。在选定条件下全血中甲胺磷、乙酰甲胺磷的线性范围为2～200ng/ml,最小定量限为2ng/ml。结论将全血样品进行直接稀释并应用液相色谱-质谱法进行检测可作为甲胺磷及乙酰甲胺磷中毒的快速检测方法。     

ABO基因分型与多重STR联合检测在法医学中的应用

目的建立ABO基因型和Goldeneye16A试剂盒联合检测的方法,并评价其在法医学实践中的应用价值。方法将6种ABO基因型(A/A,A/O,B/B,B/O,A/B,O/O)的序列特异性引物(PCR-SSP)检测方法与Goldeneye16A试剂盒相整合进行同步分型。通过对460份男性个体血痕样本、9947A DNA及90份案件样本进行检测,考察方法的一致性、灵敏度及对法庭科学检材的适用性。结果应用本文方法可同时检出6种ABO基因型和15个常染色体STR基因座及性别决定基因座,检测灵敏度为125pg,其中ABO基因检测灵敏度达63pg。460份男性血痕和90份案件检材证实该联合分型方法用于各类检材结果准确、稳定。结论本文ABO基因分型与多重STR联合检测方法,适用于各类含有核细胞的生物检材,在法庭科学DNA鉴定中有较好的应用前景。     

The Measurement of Stable Carbon Isotope Ratios of Eight Methamidophos Samples

Between December 2007 and January 2008, people suffered from food poisoning in the Japanese prefectures of Chiba and Hyogo after eating frozen dumplings (gyoza) produced in China, which had very high concentrations (1490–19,290 ppm) of methamidophos (O,S‐dimethyl phosphoramidothioate). Thus, we measured the stable carbon isotope ratio of methamidophos using GC/C/IRMS to identify the source. We analyzed seven methamidophos reagents and one Chinese agricultural methamidophos chemical (MTD600) that contained many impurities. The δ¹³C values of the seven methamidophos reagents and MTD600 ranged from ?49.23‰ to ?31.90‰, with an average SD of 0.20‰, very high precision. This difference (17.33‰) was very large compared with that in previous reports and may be attributable to the material itself and the chemical processing of methamidophos. Criminals can easily obtain pesticides such as methamidophos; therefore, it is very important to identify the pesticide source and distribution route using stable isotopic science in the future.     

甲胺磷在家兔血保存标本中的分解动力学研究

研究甲胺磷中毒死的检血在保存中的甲胺磷分解动力学。甲胺磷中毒死的家兔血分别在室温（12～25℃）及冰箱（4℃）保存,并用气相色谱－火焰光度检测器测定不同时间的浓度。在室温及冰箱中,甲胺磷在家兔血保存标本中的分解初始很快,随时间延长,分解趋于缓。队分解曲线类似动力学静注二室模型。甲胺磷在室温保存组中的分解较冰箱中快。该研究为正确判断甲胺磷中毒的分析结果提供了参考依据。     

Acephate in biological fluids of two autopsy cases after ingestion of the chemical

Two autopsy cases, where the individuals were suspected of having ingested acephate, an organophosphorous insecticide, are reported. Acephate and its active metabolite, methamidophos (MP), were analyzed in the biological fluids by GC/MS, using the salting out method with liquid-liquid extraction columns. The first case was that of a 70-year-old man whose blood acephate was 149 microg/mL, and MP was 3.0 microg/mL. Serum pseudocholinesterase (ChE) activity was inhibited. No remarkable finding of injury or disease was determined as the cause of his death, but acute poisoning by acephate was mostly suspected. The second case was that of a 60-year-old man. A deep gash in the left neck injured the left common carotid artery in addition to the severely ischemic state of the primary organs. His blood acephate was 46 microg/mL, and MP was not detected. ChE activity was in the normal range. Hemorrhage was mainly suspected as the cause of his death. The concentrations of acephate and MP in human blood after oral ingestion are first reported here, and the acute toxic level of acephate is discussed.     

Quantitative analysis of tropane alkaloids in biological materials by gas chromatography-mass spectrometry

A simple and rapid method for quantitation of tropane alkaloids in biological materials has been developed using an Extrelut column with gas chromatography-mass spectrometry (GC-MS). Biological materials (serum and urine) were mixed with a borate buffer and then applied to an Extrelut column. The adsorbed tropane alkaloids were eluted with dichloromethane before a GC-MS analysis. Atropine-d(3) was used as an internal standard. The extracted tropane alkaloids were converted to trimethylsilyl derivatives prior to GC analysis, to improve the instability of tropane alkaloids from heating and the property of them for a GC column. The recoveries of the compounds, which had been spiked to biological materials, were more than 80%. The GC separation of the derivatives from endogenous impurities was generally satisfactory with the use of a semi-polar capillary column. Tropane alkaloids showed excellent linearity in the range of 10-5000 ng/ml and the limit of detection was 5.0 ng/ml for biological materials. The present method is simple and more rapid than those previously reported, and was applied to a poisoning case. It is useful for the routine analysis of tropane alkaloids in cases of suspected tropane alkaloids poisoning.     

高效液相色谱法测定生物体液中百草枯

目的建立HPLC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,水溶性正相液相色谱分析,结合保留时间和紫外光谱对样品中百草枯进行定性。结果经该方法测得百草枯的最小检出限为10ng/m l血(S/N≥3),线性范围为0.1~10μg/ml。结论该方法快速、灵敏、准确,能有效祛除复杂生物基质中杂质干扰,使待测组分获得满意的峰形,适用于生物检材中百草枯的分析。     

甲胺磷在犬体内的死后分布

目的建立甲胺磷的犬灌胃染毒致死模型,观察甲胺磷在犬体内的死后分布规律。方法犬经8倍LD50（7.4mg/kg）剂量甲胺磷灌胃后,观察其中毒症状,死亡后即刻解剖,分别取心、肝、脾、肺、肾、脑、右上肢肌、右下肢肌、胸肌、胃组织、心血、胆汁、玻璃体液和尿液,GC/MS和GC法检测其中甲胺磷含量。结果犬8倍LD50甲胺磷灌胃染毒后20min内出现中毒症状（,53.3±14.1）min死亡。各组织脏器及体液中甲胺磷含量由高到低分别为胃（99.84±0.87）μg/g、脾（46.87±28.67）μg/g、肝（43.82±22.74）μg/g、肾（43.79±29.04）μg/g、心血（35.36±13.98）μg/mL、肺（35.25±18.59）μg/g、尿34.81μg/mL、胸肌（19.23±17.18）μg/g、右上肢（16.92±8.98）μg/g、心（15.09±6.11）μg/g、右下肢（12.83±7.63）μg/g、脑（10.91±4.13）μg/g、胆汁（6.75±1.45）μg/mL、玻璃体液（6.22±4.97）μg/mL。结论甲胺磷在犬体内死后分布不均,胃、脾、肝、肾、心血、肺、尿检材中含量较高,可作为疑似甲胺磷中毒毒物分析的检材。     

固相萃取-GC/MS法检测生物检材中的百草枯

目的采用固相萃取-气相色谱/质谱分析方法检测血液、尿液和脏器组织中的百草枯。方法人血液、尿液和猪肺组织样品经三氯乙酸去除蛋白后,取上清用十二烷基三甲基溴化铵和十二烷基硫酸钠处理过的C18小柱提取,提取物用硼氢化钠在碱性条件下还原,产物用气相色谱/质谱法分析,外标法定量。结果生物检材中百草枯回收率为78%～87%,最低检出限为0.1μg/mL,在0.5～1mg/mL范围内线性关系良好,可对实际案例检材进行定量检测。结论本文固相萃取-气相色谱/质谱分析方法能满足中毒生物检材检验及临床毒物检验需要。     

An express immunological method for detection of human seminal plasma.

Monoclonal antibodies (Mabs) against human seminal plasma (HSP) were produced and during screening procedures dissociation constants of the antigen/antibody complexes were determined. Mab 1E5 was selected for further studies because of its high reactivity in an enzyme-linked immunoassay (ELISA) and high affinity for its corresponding antigen. The specificity of Mab 1E5 was checked in absorption ELISA with human organ extracts and some biological secretions. It was established that the 1E5-corresponding epitope was a thermostable peptide moiety which could be detected in HSP, only. This monoclonal antibody was used for the development of an express method for detection of human semen. The assay was applied for screening of 57 cases of suspected rape. A complete correlation was found between the results obtained by the proposed test and by routine microscopic methods. The newly designed immunoassay is reliable, it is easily performed and it is less time-consuming.