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The Detection of THCA Using 2-Dimensional Gas Chromatography-Tandem Mass Spectrometry in Human Fingernail Clippings: Method Validation and Comparison with Head Hair
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作者 Joseph Jones Mary Jones +1 位作者 Charles Plate Douglas Lewis 《American Journal of Analytical Chemistry》 2013年第10期1-8,共8页
Marijuana use as well as abuse is a significant public health and public safety concern in the United States and using hair to identify marijuana users and abusers has been gaining acceptance in a number of venues inc... Marijuana use as well as abuse is a significant public health and public safety concern in the United States and using hair to identify marijuana users and abusers has been gaining acceptance in a number of venues including workplace, court ordered, and substance abuse treatment monitoring. After the presentation of a fully validated 2-dimensional gas chromatography-tandem mass spectrometry method for the detection of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCA), the chief metabolite of the main psychoactive compound in marijuana, Δ9-tetrahydrocannabinol (THC), we evaluated the usefulness of fingernail clippings as an alternative specimen type to hair by the analysis of a set of 60 matched pairs of head hair and fingernail clippings. The limit of detection was 10 fg/mg, the limit of quantitation was 20 fg/mg, and the assay was linear from 20 fg/mg to 500 fg/mg. The intra- and inter-assay imprecision and bias studies at 4 different concentrations (50, 100, 500, and 1000 fg/mg) were acceptable where all % Target observations were within 16% of their expected concentrations and all %CV calculations were less than 13.5%. THCA was detectable in more fingernail specimens (53.3%) than hair specimens (46.7%) and the mean concentrations in nails were on average 4.9 times higher than in hair (1813 fg/mg and 364 fg/mg, respectively). The THCA concentrations in hair and nail were strongly associated (r = 0.974, P < 0.01, n = 60) and the association was significant. The study demonstrated that fingernail clippings are a suitable alternative specimen type to hair to monitor for marijuana use and abuse. 展开更多
关键词 11-Nor-9-Carboxy-Δ9-Tetrahydrocannabinol THCA Carboxy-THC HAIR Fingernail 2D-GC-MS/MS 2-dimensional Gas chromatography Tandem mass spectrometry
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气相色谱-质谱联用法和气相色谱法对多功能控暴剂中臭味气体的定性、定量分析 被引量:4
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作者 张兴高 马士洲 +3 位作者 程万影 安文书 郝雪颖 卢薇 《理化检验(化学分册)》 CAS CSCD 北大核心 2018年第9期1011-1014,共4页
采用气相色谱-质谱联用法对含叔丁基硫醇、二乙基硫醚、邻氯苯亚甲基丙二腈等多种组分的多功能控暴剂进行了定性分析,实现了各物质的完全分离和各色谱峰的归属确认。使用注射器配气法实现了标准气的配制,并采用气相色谱法对多功能控暴... 采用气相色谱-质谱联用法对含叔丁基硫醇、二乙基硫醚、邻氯苯亚甲基丙二腈等多种组分的多功能控暴剂进行了定性分析,实现了各物质的完全分离和各色谱峰的归属确认。使用注射器配气法实现了标准气的配制,并采用气相色谱法对多功能控暴剂中叔丁基硫醇进行定量分析。叔丁基硫醇气体样品的质量浓度在5~1 000μg·L^(-1)内与其对应的峰高呈线性关系,进样量为1mL时,检出限(3S/N)为5μg·L^(-1)。加标回收率在97.2%~105%之间,对同一样品连续进样测定,测定值的相对标准偏差(n=6)为3.2%。 展开更多
关键词 气相色谱法 气相色谱-质谱联用法 叔丁基硫醇 二乙基硫醚 邻氯苯亚甲基丙二腈 臭味气体
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在线液相-气相二维色谱-质谱联用法测定烟用香精和料液中苯并[a]芘的含量 被引量:2
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作者 叶灵 熊文 +6 位作者 张承明 范多青 芮晓东 缪明明 刘志华 杨光宇 秦云华 《理化检验(化学分册)》 CAS CSCD 北大核心 2017年第1期1-5,共5页
样品10.0g,加水10mL稀释,加0.100g·L-1 D12-苯并[a]芘内标溶液200μL,加环己烷10mL,以20 000r·min-1速率漩涡振荡萃取5min。提取液直接进入液相色谱,经微型硅胶柱分离净化,含苯并[a]芘的部位切割进入气相色谱,经毛细管柱分离... 样品10.0g,加水10mL稀释,加0.100g·L-1 D12-苯并[a]芘内标溶液200μL,加环己烷10mL,以20 000r·min-1速率漩涡振荡萃取5min。提取液直接进入液相色谱,经微型硅胶柱分离净化,含苯并[a]芘的部位切割进入气相色谱,经毛细管柱分离后进入质谱分析,采用选择离子监测模式(SIM)进行测定。苯并[a]芘的质量浓度在0.08~50ng·L-1范围内与峰面积呈线性关系,方法的检出限(3s)为0.12ng·g-1,在3个不同浓度水平上进行了回收试验,回收率在92.7%~98.1%之间,测定值的相对标准偏差(n=7)在3.2%~3.7%之间。 展开更多
关键词 在线液相-气相二维色谱 苯并[A]芘 烟用香精和料液
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