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薄荷协议:气相色谱-离子迁移谱法的初步结果。

Peppermint protocol: first results for gas chromatography-ion mobility spectrometry.

机构信息

Centre for Analytical Science, Department of Chemistry, Loughborough University, Loughborough, United Kingdom.

British Columbia Cancer Research Institute, Vancouver, British Columbia, Canada.

出版信息

J Breath Res. 2022 May 26;16(3). doi: 10.1088/1752-7163/ac6ca0.

Abstract

Theseeks to inform the standardisation of breath analysis methods. Fivewith gas chromatography-ion mobility spectrometry (GC-IMS), operating in the positive mode with a tritiumH 5.68 keV, 370 MBq ionisation source, were undertaken to provide benchmarkdata for this technique, to support its use in breath-testing, analysis, and research. Headspace analysis of a peppermint-oil capsule by GC-IMS with on-column injection (0.5 cm) identified 12 IMS responsive compounds, of which the four most abundant were: eucalyptol;-pinene;-pinene; and limonene. Elevated concentrations of these four compounds were identified in exhaled-breath following ingestion of a peppermint-oil capsule. An unidentified compound attributed as a volatile catabolite of peppermint-oil was also observed. The most intense exhaled peppermint-oil component was eucalyptol, which was selected as a peppermint marker for benchmarking GC-IMS. Twenty-five washout experiments monitored levels of exhaled eucalyptol, by GC-IMS with on-column injection (0.5 cm), at= 0 min, and then at+ 60,+ 90,+ 165,+ 285 and+ 360 min from ingestion of a peppermint capsule resulting in 148 peppermint breath analyses. Additionally, thedata was used to evaluate clinical deployments with a further five washout tests run in clinical settings generating an additional 35 breath samples. Regression analysis yielded an average extrapolated time taken for exhaled eucalyptol levels to return to baseline values to be 429 ± 62 min (±95% confidence-interval). The benchmark value was assigned to the lower 95% confidence-interval, 367 min. Further evaluation of the data indicated that the maximum number of volatile organic compounds discernible from a 0.5 cmbreath sample was 69, while the use of an in-line biofilter appeared to reduce this to 34.

摘要

本研究旨在为呼吸分析方法的标准化提供信息。采用五台气相色谱-离子迁移谱(GC-IMS),以正模式运行,使用氚 5.68keV、370MBq 的电离源,为该技术提供基准数据,支持其在呼吸测试、分析和研究中的应用。通过 GC-IMS 对薄荷油胶囊的顶空分析,采用柱上进样(0.5cm),鉴定出 12 种对 IMS 有响应的化合物,其中含量最丰富的四种为:桉油醇;-蒎烯;-蒎烯;和柠檬烯。摄入薄荷油胶囊后,呼出气体中这四种化合物的浓度升高。还观察到一种被认为是薄荷油挥发性代谢物的未识别化合物。呼出薄荷油中最强的成分是桉油醇,被选为基准 GC-IMS 的薄荷油标记物。25 次洗脱实验通过 GC-IMS 柱上进样(0.5cm)监测呼出桉油醇的水平,在=0min 时进行,然后在摄入薄荷胶囊后+60、+90、+165、+285 和+360min 时进行,共进行了 148 次薄荷呼吸分析。此外,还使用该数据在临床环境中进行了另外 5 次洗脱测试,共生成了 35 个额外的呼吸样本,对临床部署进行了评估。回归分析得出,呼出桉油醇水平恢复到基线值所需的平均外推时间为 429±62min(±95%置信区间)。基准值被分配给置信区间下限,即 367min。对数据的进一步评估表明,从 0.5cm 呼吸样本中可识别的挥发性有机化合物的最大数量为 69,而使用在线生物过滤器似乎将其减少到 34。

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