Validated method for the simultaneous determination of Δ-THC and Δ-THC-COOH in oral fluid, urine and whole blood using solid-phase extraction and liquid chromatography–mass spectrometry with electrospray ionization

A fully validated, sensitive and specific method for the extraction and quantification of Δ⁹-tetrahydrocannabinol (THC) and 11-nor-9-carboxy-Δ⁹-THC (THC-COOH) and for the detection of 11-hydroxy-Δ⁹-THC (11-OH THC) in oral fluid, urine and whole blood is presented. Solid-phase extraction and liquid chromatography–mass spectrometry (LC–MS) technique were used, with electrospray ionization. Three ions were monitored for THC and THC-COOH and two for 11-OH THC. The compounds were quantified by selected ion recording of m/z 315.31, 329.18 and 343.16 for THC, 11-OH THC and THC-COOH, respectively, and m/z 318.27 and 346.26 for the deuterated internal standards, THC-d₃ and THC-COOH-d₃, respectively. The method proved to be precise for THC and THC-COOH both in terms of intra-day and inter-day analysis, with intra-day coefficients of variation (CV) less than 6.3, 6.6 and 6.5% for THC in saliva, urine and blood, respectively, and 6.8 and 7.7% for THC-COOH in urine and blood, respectively. Day-to-day CVs were less than 3.5, 4.9 and 11.3% for THC in saliva, urine and blood, respectively, and 6.2 and 6.4% for THC-COOH in urine and blood, respectively. Limits of detection (LOD) were 2 ng/mL for THC in oral fluid and 0.5 ng/mL for THC and THC-COOH and 20 ng/mL for 11-OH THC, in urine and blood. Calibration curves showed a linear relationship for THC and THC-COOH in all samples (r² > 0.999) within the range investigated.The procedure presented here has high specificity, selectivity and sensitivity. It can be regarded as an alternative method to GC–MS for the confirmation of positive immunoassay test results, and can be used as a suitable analytical tool for the quantification of THC and THC-COOH in oral fluid, urine and/or blood samples.     

SPME结合衍生化检测尿液中吗啡成份

目的　建立尿液中吗啡检验的方法。方法　利用固相微萃取头富集尿液中吗啡 ,经醋酸酐衍生后进行GC/MS分析。结果　利用此方法可检测到吗啡含量为 5ug/ml的尿样。结论　该方法可用于吸毒人员尿液中吗啡的快速检验。     

尿素中毒的检验

目的　建立了用气质联用法定量分析尿素的方法。　方法　采用传统滴定分析和气质联用定性定量检验对照分析。　结果　在 0 1μg～ 5 0 μg范围内 ,该方法有较好的线性 (r >0 9976 )。　 结论　该方法准确、快速 ,适用于尿素的定量分析     

生物样品中鸦片类毒品检验概述

概述了近 5年来生物样品中鸦片类毒品的检验情况 ,其中包括鸦片类毒品的主要种类及结构 ,鸦片类毒品在体内的代谢 ,LLE、SPE和SFE等提取净化技术 ,免疫测定、GC/MS、HPLC和LC/MS等检测方法。     

Drugs in oral fluid in randomly selected drivers

There were 13,176 roadside drug tests performed in the first year of the random drug-testing program conducted in the state of Victoria. Drugs targeted in the testing were methamphetamines and Δ⁹-tetrahydrocannabinol (THC). On-site screening was conducted by the police using DrugWipe^®, while the driver was still in the vehicle and if positive, a second test on collected oral fluid, using the Rapiscan^®, was performed in a specially outfitted “drug bus” located adjacent to the testing area. Oral fluid on presumptive positive cases was sent to the laboratory for confirmation with limits of quantification of 5, 5, and 2 ng/mL for methamphetamine (MA), methylenedioxy-methamphetamine (MDMA), and THC, respectively. Recovery experiments conducted in the laboratory showed quantitative recovery of analytes from the collector. When oral fluid could not be collected, blood was taken from the driver and sent to the laboratory for confirmation. These roadside tests gave 313 positive cases following GC–MS confirmation. These comprised 269, 118, and 87 cases positive to MA, MDMA, and THC, respectively. The median oral concentrations (undiluted) of MA, MDMA, and THC was 1136, 2724, and 81 ng/mL. The overall drug positive rate was 2.4% of the screened population. This rate was highest in drivers of cars (2.8%). The average age of drivers detected with a positive drug reading was 28 years. Large vehicle (trucks over 4.5 t) drivers were older; on average at 38 years. Females accounted for 19% of all positives, although none of the positive truck drivers were female. There was one false positive to cannabis when the results of both on-site devices were considered and four to methamphetamines.     

利用GC／MS检验致幻剂麦角酰二乙胺

目的建立检验致幻剂麦角酰二乙胺的方法。方法用气相色谱与质谱联用仪(GC/MS)进行定性分析。结果麦角酰二乙胺质谱图保留时间为19.683min。结论该方法用于检案简单、可靠。     

GC／MS分析鱼塘水中的五氯酚

目的介绍GC/MS分析鱼塘水中五氯酚的方法。方法将约500ml鱼塘水调至pH=3,用约50ml苯萃取、无水硫酸钠干燥过滤、浓缩至约0.2ml,然后再利用GC/MS联用仪分析。结果用该方法检验出四氯苯酚和五氯苯酚。结论这种方法可用来对鱼塘投毒案件中的水样进行五氯酚的检验。     

GC/MS立体选择性分析人尿和肝中d-甲基苯丙胺对映体

建立的d-和1－MP的立体选择性GC／MS分析方法，以1－TPC为手性酸化试剂，将MP转变为相应的酸胺类非对映体对，于常规非CSP上分离。该法灵敏度高，并具有宽的线性范围（10～2000ng／mLr＞0．999n=8）。尿中存在的是d-还是1－MP将有助于判断MP的来源。本案例尿样中心MP浓度比1-MP高11倍，肝组织中也接近10倍，提示滥用了违法药品d－MP。     

The de Bunsen Committee and a revision of the ‘conspiracy’ of Sykes–Picot

The Sykes–Picot The Sykes-Picot Agreement is often cited as evidence of a Western conspiracy to carve up the Middle East and subordinate the Arabs. It is a prevalent view across the region, and has been a refrain repeated by critics. Yet very little is known of the far more significant conclusions of a Committee, formed by Maurice de Bunsen on the orders of the British government, which ascertained the options open to the Allies in 1915. Far from a nefarious conspiracy, the Committee came down in favour of a decentralised, ultimately independent region. The First World War compelled some revision of the original intent, but the essence of the Committee's conclusions remained intact throughout the war, and after. Conversely, Sir Mark Sykes repudiated the ‘agreement’ he had made with the French diplomat Picot, and substantial revisions were made to that temporary scheme. Yet it seems that ‘conspiracy sells’, and generations have colluded with the theme of perfidy to reinforce particular narratives, including, most recently, the Da´esh movement's claim to have ‘ended Sykes-Picot’.     

Explaining Canada–US differences in attitudes toward the role of government: a test of S.M. Lipset’s ‘Continental Divide’

For decades scholars have engaged in a lively debate about the distinctiveness of Canadian and American value systems. Lipset (1990) argues that divergent responses to the American Revolution led Canada to embrace Tory values of ‘peace, order, and good government’ while Americans pursued classical liberal values of ‘life, liberty, and the pursuit of happiness’. Other scholars question the extent, or even the existence, of the differences Lipset describes. Using surveys of students from Canadian and American universities close to the Canada–US border, we identify compelling support for Lipset’s hypothesised differences on the role of government in the least likely setting imaginable.