新型固相萃取技术在刑事毒物分析中的应用

发布时间：2018-11-09 08:02

【摘要】：随着分析技术的不断发展进步,各种先进的仪器分析方法不断被引入刑事毒物分析实践中,取得了重大突破。但由于刑事案件中毒物分析的检材及毒物种类的多样性,在大多数情况下,都必须对检材进行前处理,以满足仪器检测的要求,发展新型前处理技术是刑事毒物分析的迫切需要。本文将经C18表面改性的磁性纳米颗粒Fe3O4@SiO2作为基质固相分散萃取吸附剂,用于大体积水样中农药和尿样中安眠药的萃取,并结合气相色谱-质谱(GC/MS)进行检测。系统考察了磁性纳米颗粒用量、洗脱剂种类和用量、萃取时间等条件对回收率的影响。优化后,农药组分最高富集倍数达到1015倍。将优化的方法用于投毒案中池塘水的检验,检出乐果和氯氰菊酯成分,浓度分别为9.0ng/L和16ng/L。实验证明,将磁性纳米材料直接分散在水中,快速磁分离后即完成萃取,操作简便、重复性好、回收率高、富集倍数高、检出限低,能满足水样中低浓度组分检测的要求。利用全自动固相萃取系统从人的血液检材中提取三大类(九种)不同种类的常见安眠镇静药物,然后采用气相色谱-离子阱二级质谱(GC/MS/MS)对目标药物进行定性、定量检测分析。将建立的优化方法应用于实际案例中的人心血中安眠镇静药物的定性及定量检测,检出安定成分且其含量为0.6μg/mL。分别采用超声辅助固相萃取和常规液液萃取提取蔬菜中残留的有机磷农药成分,结合GC/MS/MS对九种有机磷农药进行定性和定量检测。所建立的方法简单,快速,灵敏度高。
[Abstract]:With the continuous development and progress of analytical technology, various advanced instrument analysis methods have been continuously introduced into the criminal toxicological analysis practice, which has made a great breakthrough. However, due to the diversity of samples and types of poisons analyzed in criminal cases, in most cases, the samples must be pre-treated to meet the requirements of instrument testing. The development of new pre-treatment technology is an urgent need for the analysis of criminal poisons. In this paper, the magnetic nanoparticles Fe3O4@SiO2 modified by C18 surface were used as matrix solid phase dispersion extraction adsorbent for extraction of pesticides in bulk water and sleeping pills in urine, and were detected by gas chromatography-mass spectrometry (GC/MS). The effects of the amount of magnetic nanoparticles, the type and amount of eluent and extraction time on the recovery were systematically investigated. After optimization, the maximum enrichment ratio of pesticide components reached 1015 times. The optimized method was applied to the detection of dimethoate and cypermethrin in pond water of poisoning cases. The concentrations of dimethoate and cypermethrin were 9.0ng/L and 16ng / L, respectively. The experiment shows that the magnetic nanomaterials are dispersed directly in water, and the extraction is completed immediately after rapid magnetic separation, which is easy to operate, good in repeatability, high in recovery rate, high in enrichment ratio and low in detection limit, which can meet the requirements of the detection of low concentration components in water samples. Three kinds of common sedative drugs were extracted from human blood samples by automatic solid phase extraction system. Then the target drugs were qualitatively determined by gas chromatography-ion trap mass spectrometry (GC/MS/MS). Quantitative analysis. The established optimization method was applied to the qualitative and quantitative detection of asphyxiating sedatives in human heart blood. The diazepam component was detected and its content was 0.6 渭 g / mL. Ultrasonic assisted solid phase extraction (SPE) and conventional liquid-liquid extraction (liquid-liquid extraction) were used to extract organophosphorus pesticide residues from vegetables. Nine organophosphorus pesticides were determined qualitatively and quantitatively with GC/MS/MS. The method is simple, rapid and sensitive.
【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：D918;O658.2

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