GC双检测器技术筛选常见毒(药)物的可行性研究

利用气相色谱仪 ,在样品进样经单柱分离后通过Y形管连接至两个不同选择性检测器 (NPD/FID)的方法 ,考察气相色谱操作条件对双检测器响应比值的影响及其该法用于复杂样品测定的可行性。结果表明当实验条件保持不变时 ,NPD/FID响应比值具有较好的重现性。改变检测器操作参数和色谱条件对NPD/FID响应比值都有影响 ,但相对于某一参比物计算得到的相对NPD/FID响应比值受影响很小。样品中待测组份的浓度改变不影响NPD/FID响应比值。在有标准品比对的情况下 ,NPD/FID响应比值或相对NPD/FID响应比值可以作为定性分析的一个参数。     

LC／MS／MS法测定全血中马钱子碱和士的宁的含量

目的建立定量分析人全血中马钱子碱和士的宁的高效液相色谱质谱联用法。方法应用Oasis^TM MCX小柱进行固相萃取法提取，XTerra^TM RP18色谱柱分离。结果在该条件下，人血中马钱子碱和士的宁的线性范围为0．01—5．0μg／ml，最小检出限为0．2ng／ml；马钱子碱和士的宁在0．01—5．0μg／ml浓度范围内的回收率均在80％以上。结论高效液相色谱质谱联用法可定量测定血中马钱子碱和士的宁。     

公共安全中化学战剂确证的色谱分析技术

随着公共安全工作的需要，化学战剂（CWAs）的确认成功分析化学中一个重要的应用领域。色谱和质谱技术已应用于环境样品中大多数典型CWAs及其降解后产物的分析。本文综述了目前分析化学战剂的各类检测技术。     

毒鼠强与马钱子碱混合毒物的GC/MS检验分析

毒鼠强（Tetramine，化学结构式见图1）又名“424”、鼠没命等，化学名为四次甲基二砜四胺，分子式：C4H8N4O4S2，分子量：240．27，纯品为白色粉末，255℃～260℃分解，无味，不溶于水，难溶于乙醇，可溶于丙酮、氯仿、苯等有机溶剂。毒鼠强的毒性很大，入口服最低致死量为5mg／Kg.     

The Identification of Ingested Dandelion Juice in Gastric Contents of a Deceased Person by Direct Sequencing and GC–MS Methods*

Abstract: DNA and chemical analysis of gastric contents of a deceased person were handled in this work. The body of the victim was discovered in his car, submerged in a lake. We were asked to determine whether or not the gastric contents of the victim harbored drugs and dandelion material. It was suspected that the victim had been murdered by poisoning with an excess amount of sleeping medication (doxylamine), which had been homogenized with dandelion. The concentrations of 11.4 and 27.5 mg/kg of doxylamine detected from spleen and liver of the victim were far higher than the assumed therapeutic concentration. Via gas chromatography–mass spectrometry (GC–MS) analysis and direct sequencing analysis of plant genetic markers such as intergenic transcribed spacer, 18S ribosomal RNA (rRNA), rbcL and trnLF, it was confirmed that the gastric contents of the victim contained taraxasterol, which is one of the marker compounds for dandelion and contained dandelion species‐specific rbcL and trnL‐trnF IGS (trnLF) sequences. The initial PCR of the genomic DNA isolated from the gastric contents showed insufficient quantity, and the second PCR, of which the template was a portion of the initial PCR products, exhibited a sufficient quantity for direct sequencing. rbcL and trnLF located in the cpDNA resulted in the successful determination of dandelion DNA in a decedent’s stomach contents. GC–MS identifies the actual presence of a taraxasterol at 28.4 min. Raw dandelion was assumed to be used as a masking vehicle for excess sleeping drug (doxylamine).     

微波萃取和PTV—GC／MS／MS结合分析血中常见有机磷农药

微波萃取技术是80年代中期开始发展起来的一种新的萃取技术，他具有选择性好、加热效率高、萃取结果不受物质水分含量影响，回收率高、试剂用量少、处理批量大，萃取效率高等优点，微波萃取被誉为“绿色分析化学”。微波萃取技术现已广泛应用到土壤分析、化工、食品、香料、中草药和化妆品等领域，但血中有机磷农药的提取技术还未曾报道。作者利用此技术萃取血中的常见有机磷农药，为排查血液中的毒物提供了一种新的方法。     

Determination of ibogaine and noribogaine in biological fluids and hair by LC-MS/MS after Tabernanthe iboga abuse Iboga alkaloids distribution in a drowning death case

Tabernanthe iboga belongs to the Apocynaceae family. In this study, we report the case of a 37-year-old black male working as a security agent in Paris and found dead naked on the beach in Gabon after consumption of iboga. Autopsy revealed a drowning fatality and a myocardial abnormality (myocardial bridging). Samples of blood, urine, bile, gastric content, liver, lungs, vitreous, spleen and hair were taken. Biological fluids were liquid-liquid extracted with saturated NH4Cl pH 9.5 and methylene chloride/isopropanol (95/5, v/v) in presence of clonazepam-d(4), used as internal standard. After decontamination with dichloromethane, hair was cut into small pieces then sonicated for 2h in saturated NH4Cl pH 9.5 before extraction by methylene chloride/isopropanol (95/5, v/v). After evaporation the residues were reconstituted in methanol/ACN/formate buffer pH 3, from which 10 microL were injected into an ODB Uptisphere C(18) column (150 mm x 2.1mm, 5 microm) and eluted with a gradient of acetonitrile and formate buffer delivered at a flow rate of 200 microL/min. A Quantum Ultra triple-quadrupole mass spectrometer was used for analyses. Ionization was achieved using electrospray in the positive ionization mode (ESI). For each compound, detection was related to three daughter ions (ibogaine: m/z 311.4-->122.1, 174.1 and 188.1; noribogaine: m/z 297.4-->122.1, 159.1 and 160.1; clonazepam-d(4): m/z 319.9-->218.1, 245.1 and 274.1). Ibogaine and noribogaine were detected in all autopsy samples. Hair segmentation was not possible as hair was very short and frizzy. Concentrations of 1.2 and 2.5 ng/mg, respectively were detected. Neither other licit or illicit drugs nor alcohol were found. The presence of ibogaine and noribogaine in all autopsy samples was consistent with the recent absorption of Tabernanthe iboga, which was assumed to be responsible of the drowning fatality. The history of exposure, regarding hair analysis, is discussed. LC-MS/MS appears to be the best method for analyzing complex and poorly volatile alkaloids in autopsy samples and particularly in hair, due to the presence of a nitrogen ring and the relatively low concentrations to be measured.     

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。     

气相色谱-串联质谱法测定血液中乙基葡萄糖醛酸苷

目的建立血液中乙基葡萄糖醛酸苷（ethyl glucuronide,EtG）的气相色谱-串联质谱（GC-MS/MS）测定方法。方法血液用乙腈沉淀蛋白,离心后,将上清液转移吹干,残留物经N,O-双（三甲基硅烷基）三氟乙酰胺衍生化,用GC-MS/MS进行检测。结果血液中EtG的检出限为0.05μg/mL,线性范围为0.1～10μg/mL（r=0.9999）。对送检案例血液检材进行EtG检测,效果良好。结论本方法适用于血液中EtG的检测。     

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。