Jack Henion, Changtong Hao, Daniel Eikel, Olof Beck, Peter Stambeck
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A simple one-step ethanol extraction of the “A” breath collector sample can be analyzed by UHPLC/selected ion monitoring (SIM) liquid chromatography/mass spectrometry (LC/MS) to provide qualitative and quantitative determination of THC in breath sample in less than 4 min for samples collected up to 6 h after smoking a cannabis cigarette. SIM LC/MS bioanalyses employed d3-THC as the stable isotope internal standard fortified in negative control breath samples for quantitation including replicates of six calibrator standards and three quality control (QC) samples. Subsequent confirmation of the same breath sample in the B collectors was then confirmed by a reference lab by LC/MS/MS analysis. Fit-for-purpose bioanalytical validation consistent with pharmaceutical regulated bioanalyses produced pharmacokinetic (PK) curves for the two volunteer cannabis smokers. These results produced PK curves, which showed a rapid increase of THC in the breath of the subjects in the first hour followed by reduced THC levels in the later time points. A simpler single-point calibration curve procedure with calibrators and QC prepared in ethanol provided similar results. Limitations to this approach include the higher cost and operator skill sets for the instrumentation employed and the inability to actually determine driver impairment.</p>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.9000,"publicationDate":"2023-12-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"An analytical approach for on-site analysis of breath samples for Δ9-tetrahydrocannabinol (THC)\",\"authors\":\"Jack Henion, Changtong Hao, Daniel Eikel, Olof Beck, Peter Stambeck\",\"doi\":\"10.1002/jms.4987\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>Increased acceptance of cannabis containing the psychoactive component, Δ9-tetrahydrocannabinol (THC), raises concerns about the potential for impaired drivers and increased highway accidents. 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SIM LC/MS bioanalyses employed d3-THC as the stable isotope internal standard fortified in negative control breath samples for quantitation including replicates of six calibrator standards and three quality control (QC) samples. Subsequent confirmation of the same breath sample in the B collectors was then confirmed by a reference lab by LC/MS/MS analysis. Fit-for-purpose bioanalytical validation consistent with pharmaceutical regulated bioanalyses produced pharmacokinetic (PK) curves for the two volunteer cannabis smokers. These results produced PK curves, which showed a rapid increase of THC in the breath of the subjects in the first hour followed by reduced THC levels in the later time points. A simpler single-point calibration curve procedure with calibrators and QC prepared in ethanol provided similar results. 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引用次数: 0
摘要
人们越来越多地接受含有精神活性成分 Δ9-四氢大麻酚(THC)的大麻,这引起了人们对驾驶者精神受损和高速公路交通事故增加可能性的担忧。人们普遍接受 "呼气式酒精测试 "来确定驾驶员体内的酒精含量,与此不同的是,目前还没有公认的路边四氢大麻酚测试方法来确定驾驶员体内的四氢大麻酚含量。因此,需要一种易于收集的生物样本,从可能受损的驾驶者身上采集,同时进行准确的现场测试,以测量驾驶者体内四氢大麻酚的存在和数量。本文介绍了一种新颖的呼气采集装置,它包括三个独立的样本采集器,分别用于从被测者身上采集相同的 A、B 和 C 呼气样本。通过超高效液相色谱/选择离子监测(SIM)液相色谱/质谱法(LC/MS)对 "A "呼气采集器样本进行简单的一步乙醇提取分析,可在 4 分钟内对吸食大麻烟后 6 小时内采集的呼气样本中的四氢大麻酚进行定性和定量测定。SIM LC/MS 生物分析采用 d3-THC 作为稳定同位素内标,在阴性对照呼气样本中进行定量,包括六个校准标准和三个质量控制(QC)样本的重复样本。随后,参考实验室通过 LC/MS/MS 分析对 B 收集器中的相同呼气样本进行确认。与制药监管生物分析一致的适合目的生物分析验证为两名自愿大麻吸食者生成了药代动力学(PK)曲线。这些结果绘制出的药代动力学曲线显示,受试者呼气中的四氢大麻酚含量在第一小时内迅速增加,随后的时间点四氢大麻酚含量有所降低。使用在乙醇中制备的校准物和质控物进行更简单的单点校准曲线程序也得到了类似的结果。这种方法的局限性包括所使用仪器的成本较高,操作人员的技能要求较高,以及无法实际确定驾驶员的损伤程度。
An analytical approach for on-site analysis of breath samples for Δ9-tetrahydrocannabinol (THC)
Increased acceptance of cannabis containing the psychoactive component, Δ9-tetrahydrocannabinol (THC), raises concerns about the potential for impaired drivers and increased highway accidents. In contrast to the “breathalyzer” test, which is generally accepted for determining the alcohol level in a driver, there is no currently accepted roadside test for THC in a motorist. There is a need for an easily collectible biological sample from a potentially impaired driver coupled with an accurate on-site test to measure the presence and quantity of THC in a driver. A novel breath collection device is described, which includes three separate sample collectors for collecting identical A, B, and C breath samples from a subject. A simple one-step ethanol extraction of the “A” breath collector sample can be analyzed by UHPLC/selected ion monitoring (SIM) liquid chromatography/mass spectrometry (LC/MS) to provide qualitative and quantitative determination of THC in breath sample in less than 4 min for samples collected up to 6 h after smoking a cannabis cigarette. SIM LC/MS bioanalyses employed d3-THC as the stable isotope internal standard fortified in negative control breath samples for quantitation including replicates of six calibrator standards and three quality control (QC) samples. Subsequent confirmation of the same breath sample in the B collectors was then confirmed by a reference lab by LC/MS/MS analysis. Fit-for-purpose bioanalytical validation consistent with pharmaceutical regulated bioanalyses produced pharmacokinetic (PK) curves for the two volunteer cannabis smokers. These results produced PK curves, which showed a rapid increase of THC in the breath of the subjects in the first hour followed by reduced THC levels in the later time points. A simpler single-point calibration curve procedure with calibrators and QC prepared in ethanol provided similar results. Limitations to this approach include the higher cost and operator skill sets for the instrumentation employed and the inability to actually determine driver impairment.
期刊介绍:
The Journal of Mass Spectrometry publishes papers on a broad range of topics of interest to scientists working in both fundamental and applied areas involving the study of gaseous ions.
The aim of JMS is to serve the scientific community with information provided and arranged to help senior investigators to better stay abreast of new discoveries and studies in their own field, to make them aware of events and developments in associated fields, and to provide students and newcomers the basic tools with which to learn fundamental and applied aspects of mass spectrometry.