法医毒物分析中有机磷农药及安定类药物GC-MS定性分析结果评判技术研究

发布时间：2018-04-22 05:15

本文选题：法医毒物分析 + 定性结果　；参考：《山西医科大学》2017年硕士论文

【摘要】：目的:1.建立人血液同时检测敌敌畏和甲拌磷的GC-MS检测方法及同时检测安定和舒乐安定的GC-MS检测方法。2.研究有机磷农药(敌敌畏、甲拌磷)及安定类药物(安定、舒乐安定)在GC-MS全扫描模式下的定性参数(保留时间、离子比率)结果的最大允许偏差来验证目前存在的指导性文件的可靠性。方法:1.检测方法:采用液液萃取法进行提取,分析不同的提取溶剂对药物回收率的影响,最后选择乙酸乙酯作为提取溶剂。2.统计学方法和其他软件:采用SPSS-20.0软件分析收集的数据。Graph Pad Prism 6绘图。结果:1.检测方法:采用GC-MS全扫模式检测有机磷农药(敌敌畏、甲拌磷内标磷酸三丁酯)及安定类药物(安定、舒乐安定内标SKF525A)。敌敌畏、甲拌磷线性范围为0.5-20.0μg/m L,R2分别为0.9989和0.9987,最低检出浓度(LOQ)分别为0.16μg/m L和0.14μg/m L;安定和舒乐安定的0.2-20.0μg/m L,R2分别为0.9987和0.9935,最低检出浓度(LOQ)分别为0.11μg/m L和0.10μg/m L。2.有机磷农药(敌敌畏、甲拌磷内标磷酸三丁酯)及安定类药物(安定、舒乐安定内标SKF525A)在GCMS-TQ8030三重四级杆气相色谱/质谱联用仪的全扫描模式下的保留时间(RT)和相对保留时间(RRT)在不同浓度均比较稳定;有机磷农药(敌敌畏、甲拌磷内标磷酸三丁酯)在7890A-5875C气相色谱/质谱联用仪的全扫描模式下的保留时间(RT)和相对保留时间(RRT)在不同浓度均比较稳定。RT的最大允许偏差为±0.05 min,RRT的最大允许偏差为±0.5%。3.有机磷农药(敌敌畏、甲拌磷内标磷酸三丁酯)及安定类药物(安定、舒乐安定内标SKF525A)在GCMS-TQ8030三重四级杆气相色谱/质谱联用仪全扫描模式下的特征离子的离子比率的参考值:79/109=0.30、185/109=0.26、145/109=0.08、121/75=0.33、97/75=0.225、231/75=0.10、283/256=0.935、221/256=0.59、165/256=0.2、205/259=0.53、293/259=0.37、239/259=0.35。有机磷农药(敌敌畏、甲拌磷内标磷酸三丁酯)在7890A-5875C气相色谱/质谱联用仪全扫描模式下的特征离子的离子比率的参考值:79/109=0.20、185/109=0.315、145/109=0.09、121/75=0.405、97/75=0.28、231/75=0.11。离子比率的最大允许偏差分别为±10%(绝对)和±25%(相对),低浓度或者低信噪比时离子比率的最大允许偏差可大至±50%(相对)。结论:1.本实验建立了同时检测人血中敌敌畏、甲拌磷、安定和舒乐安定的液液萃取方法和GC-MS的定性定量分析检测方法,可用于法医毒物分析中这几种药物中毒案件的法医学鉴定。2.血样添加敌敌畏和甲拌磷、安定和舒乐安定,RT的绝对偏差可以放宽至≤±0.05 min即3 s。血样添加RRT的相对标准为≤±0.5%。如果是低浓度的情况下,建议使用RRT。因为低浓度情况下,RRT的偏差较小,较RT更加可靠。3.血样添加特征离子的离子比率的大小与浓度和信噪比均有一定的关系,本实验就信噪比方面来讨论离子比率的偏差,血样添加特征离子的离子比率的绝对偏差的判定标准为±10%;相对偏差的判定指标为±25%,在低浓度/低信噪比情况下,相对偏差应扩大为±50%。但在实际工作中还是需要有经验的法医毒化检验师仔细核对数据,才可以得到最后的结论。
[Abstract]:Objective: 1. to establish a GC-MS detection method for the simultaneous detection of dichlorvos and phosphorous in human blood and the GC-MS detection method for simultaneous detection of diazepam and diazepam.2. to study the most qualitative parameters (retention time, ion ratio) of organophosphorus pesticides (dichlorvos, phosphorous) and diazepam (diazepam, diazepam) in the full scanning mode of GC-MS Large allowable deviations are used to verify the reliability of the existing guiding documents. Method: 1. detection methods: liquid liquid extraction is used to extract the effects of different solvents on drug recovery. Finally, ethyl acetate is selected as the.2. statistical method and other software for extracting solvent: SPSS-20.0 software is used to analyze the collected data.Gr APH Pad Prism 6 drawing. Results: 1. detection method: using GC-MS total scanning mode to detect organophosphorus pesticides (dichlorvos, phosphoric acid three butyl ester) and diazepam (diazepam, diazepam SKF525A). Dichlorvos, dichlorvos linear range is 0.5-20.0 mu g/m L, R2 is 0.9989 and 0.9987 respectively, and the lowest detection concentration (LOQ) is 0.16 mu g, respectively. /m L and 0.14 mu g/m L; 0.2-20.0 mu g/m L of diazepam and diazepam, R2 respectively 0.9987 and 0.9935, and the lowest detection concentration (LOQ) are 0.11 mu L and 0.10 micron organophosphorus pesticides (dichlorvos, phosphoric acid three butyl phosphate) and diazepam (diazepam, diazepam) in three heavy four level gas chromatography / The retention time (RT) and relative retention time (RRT) were stable at different concentrations in the full scanning mode of the mass spectrometry, and the retention time (RT) and relative retention time (RRT) of organophosphorus pesticides (dichlorvos, three butyl phosphate) in the 7890A-5875C gas chromatography / mass spectrometry combined instrument were in different concentration ratios. The maximum permissible deviation of the more stable.RT is + 0.05 min, and the maximum allowable deviation of RRT is the ratio of the characteristic ions of the characteristic ions under the full scanning mode of the GCMS-TQ8030 three heavy four grade gas chromatograph / mass spectrometry with the maximum permissible deviation of the 0.5%.3. organophosphorus pesticide (dichlorvos, the phosphoric acid phosphate) and the diazepam (diazepam and diazepam SKF525A) in the GCMS-TQ8030 three weight four grade gas chromatography / mass spectrometry. Reference values: 79/109=0.30185/109=0.26145/109=0.08121/75=0.33,97/75=0.225231/75=0.10283/256=0.935221/256=0.59165/256=0.2205/259=0.53293/259=0.37239/259=0.35. organophosphorus pesticides (dichlorvos, phosphoric acid three butyl phosphate) in the full scanning mode of 7890A-5875C gas chromatograph / mass spectrometry The reference value of the ion ratio: the maximum allowable deviation of the 79/109=0.20185/109=0.315145/109=0.09121/75=0.405,97/75=0.28231/75=0.11. ion ratio is + 10% (absolute) and + 25% (relative), the maximum allowable deviation of the ion ratio at low concentration or low signal to noise ratio can be as much as 50% (relative). Conclusion: 1. experiments have established simultaneous detection. The liquid extraction method of dichlorvos, mixed phosphorus, diazepam and diazepam in human blood and the qualitative and quantitative analysis of GC-MS can be used in forensic forensic identification of forensic toxicology, which can be used to identify.2. blood samples with dichlorvos and mixed phosphorus, diazepam and Shu Lean, and the absolute deviation of RT can be relaxed to less than 0.05 min or 3. The relative standard of S. blood sample added to RRT is less than + 0.5%. and if it is low concentration, it is suggested that using RRT. because of low concentration, the deviation of RRT is smaller and the ratio of the ion ratio added to the.3. sample more reliable than RT is related to the concentration and signal to noise ratio. This experiment discusses the ion ratio in the aspect of signal to noise ratio. The absolute deviation of the ion ratio of the blood sample is + 10%, and the determination index of the relative deviation is + 25%. The relative deviation should be expanded to + 50%. in the low concentration / low signal noise ratio, but in actual work, the empirical forensic examiner should check the data carefully before the final knot can be obtained. Theory.

【学位授予单位】：山西医科大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：D919

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