三种方法对血中氯氮平的提取

分别用乙醚、15%甲醇/乙腈混合液(15mL甲醇+85mL乙腈)、乙酸乙酯三种溶剂对血中的氯氮平进行提取,以DB-5MS石英毛细管柱、El源、不分流进样进行分析。计算回收率,比较每种溶剂提取的特点。刑事案件中时有氯氮平中毒的案件。     

错配引物诱导酶切技术检测GC多态性

目的探讨建立检测GC点突变rs7041的引物错配诱导酶切技术（mismatch primer-induced RFLP,MPIR）及应用价值。方法针对GC基因点突变（NCBI Reference SNP ID：rs7401）,设计错配引物进行PCR扩增,引物错配碱基结合GC点突变诱导XhoI酶切,产生GC-rs7041片断长度多态性,并调查183例温州汉族无关群体GC-rs7401多态性。结果引物错配诱导酶切技术对GC-rs7041亚型的3种基因型分型明确。温州地区汉族人群GC-rs7041 T/G基因频率分别为0.787和0.213,基因型频率分别为T/T0.685、T/G 0.284和G/G 0.071,Ho（0.284）、He（0.337）、PIC（0.279）、DP（0.502）、PE（0.140）,基因型分布符合Hardy-Weinberg平衡。结论成功建立引物错配诱导酶切技术检测GC-rs7041单核苷酸多态性,该位点多态性有实际应用价值。     

固相萃取法提取氟乙酸钠的实验研究

目的探讨一种氟乙酸钠的固相萃取方法。方法提取物通过与五氟苄基溴衍生化反应,用GC/MS、GC/ECD定性定量分析。结果本实验用Agilent公司的AccuBondⅡSAX柱,选择性较强,适用于氟乙酸钠的萃取;改进了去除杂质的方法,选择缓冲液pH9进行萃取,效果好,不影响回收率。结论该方法去除杂质的效果非常明显,操作简单,适合基层理化检验人员使用,并已应用于实际案例检验中。     

应用斑点酶标法检测吸毒者尿液中常见毒品

目的建立吸毒者尿液中常见毒品的斑点酶标法检测分析方法。方法生物检材为尿液,采用免疫学酶标法理论和斑点酶标法的高通量技术,应用于人体尿液中常见毒品的检测。结果同时分析多人尿液中是否含有苯丙胺、巴比妥、天使尘、美沙酮及吗啡。尿液中的最低检测量达ng级。结论本方法可用于吸毒者尿液中常见毒品的检测分析。     

Profiling the scent of weathered training aids for blood-detection dogs

At outdoor crime scenes, cadaver-detection and blood-detection dogs may be tasked with locating blood that is days, weeks or months old. Although it is known that the odour profile of blood will change during this time, it is currently unknown how the profile changes when exposed to the environment. Such variables must be studied in order to understand when the odour profile is no longer detectable by the scent-detection dogs and other crime scene tools should be implemented. In this study, blood was deposited onto concrete and varnished wood surfaces and weathered in an outdoor environment over a three-month period. Headspace samples were collected using solid phase microextraction (SPME) and analysed using comprehensive two-dimensional gas chromatography – time-of-flight mass spectrometry (GC×GC–TOFMS). The chemical odour profiles were compared with the behavioural responses of cadaver-detection and blood-detection dogs during training. Data interpretation using principal component analysis (PCA) and hierarchical cluster analysis (HCA) established that the blood odour could no longer be detected using SPME–GC×GC–TOFMS after two months of weathering on both surfaces. Conversely, the blood-detection dogs had difficulty locating the blood samples after one month of weathering on concrete and after one week of weathering on varnished wood. The scent-detection dogs evaluated herein had not been previously exposed to environmentally weathered blood samples during training. Given that this study was conducted to test the dogs' baseline abilities, it is expected that with repeated exposure, the dogs' capabilities would likely improve. The knowledge gained from this study can assist in providing law enforcement with more accurate training aids for blood-detection dogs and can improve their efficiency when deployed to outdoor crime scenes.     

安眠酮及2'-羟甲基安眠酮的毛细柱GC/MS测定

作者在 Finnigan Mat 1020 GC/MS 仪上,应用 SE-54熔融硅毛细柱,建立了生物试样中安眠酮、2'-羟甲基安眠酮的分析方法。动物中毒实验表明,此法实用,不仅能检出安眠酮,而且还可检出存在的代谢物;在实际应用中,具有快速、灵敏、准确等特点。检测限为15ng,并已用于刑事案件的鉴定工作中。     

全血中度冷丁的气—联用法测定及代谢动力学的研究

应用气－质联用选择离子法测定全血中度冷丁的浓度。方法线性范围为０．００２～１ｎｇ／ｍｌ（ｒ＝０．９９９７），变异系数小于１０％，最低检测限过１ｎｇ／ｍｌ，无杂质干扰。本法已用于肌注８０ｍｇ度冷丁后代谢动力学的研究。     

GC‐MS and IR Studies on the Six Ring Regioisomeric Dimethoxyphenylpiperazines (DOMePPs)

A number of N‐substituted piperazines have been described as drugs of abuse in recent years. This new drug category includes several series of aromatic ring substituted phenylpiperazines. The wide variety of available precursors makes regioisomerism a significant issue in these totally synthetic compounds. In this study, a complete series of regioisomeric dimethoxyphenylpiperazines were synthesized and evaluated using GC‐MS and FT‐IR. The EI mass spectra show fragments characteristic of both the dimethoxyphenyl and the piperazine portions of the molecules including the dimethoxyphenylaziridinium cation (m/z 180) and dimethoxyphenyl cation (m/z 137). The ion at m/z 56 for the C₃H₆N⁺ fragment is characteristic of the piperazine ring and was observed in all the spectra. The perfluoroacyl derivatives were resolved by GC, and their mass spectra showed some differences in relative abundance of ions. FTIR provides direct confirmatory data for differentiation between the regioisomeric dimethoxyphenylpiperazines, and GC separation was accomplished on an Rtx‐200 phase.     

硫化氢中毒者血中硫化氢的检测及特征鉴别

目的探讨硫化氢(H2S)中毒者血中H2S的检测及特征鉴别;方法取新鲜空白血液和5℃下保存1月、1年的血液各2m L,经微波低火加热1min后,吸取顶空气体100μL进行GC/PFPD-S、GC/MS检测;取相同样本进行酸化处理后进行检测;取疑似为H2S中毒者血液直接加热后进行检测。结果新鲜血液和5℃下保存1月、1年的血液均可检出H2S成分,但保存1个月以上的血液可同时检出二硫化碳(CS2)成分;酸化处理后的血液,H2S和CS2成分检出的含量明显比未加酸化的血液高;中毒者血液中除了检出H2S成分外,还检出甲硫醚成分。结论血液样本同时检出H2S和较大量的CS2时,不宜判定为H2S中毒,提示可能为腐败所致,而同时检出H2S和较大量的甲硫醚,则可做出H2S中毒的判断。     

GC/MS、GC/NPD法检测毛发中的氯胺酮

目的采用液-液萃取、衍生化和GC/MS、GC/NPD方法,进行毛发中氯胺酮定性定量分析。方法选择4-苯基丁胺为内标,毛发样本用NaOH、HCl及芳基硫酸酯酶/β-葡萄糖醛酸酶等3种方式进行水解,再进行衍生化后,采用GC/MS和GC/NPD方法定性定量分析。对不同水解和衍生化条件以及提取溶剂进行比较优化,并考察方法精密度、稳定性和检出限。结果方法的提取回收率大于95%,精密度和样品稳定性良好,日内和日间标准偏差小于6%;采用GC/NPD和GC/MS直接分析毛发中的氯胺酮,检出限为0.2ng/mg和2.0ng/mg,线性范围为10.0～250.0ng/mg,相关系数均大于0.99;采用酰化衍生化后分析,GC/NPD和GC/MS检出限分别提高至0.1ng/mg和0.2ng/mg。结论该方法回收率高、检测限低,可以用于毛发中氯胺酮的定性定量分析检验。