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Rapid Analysis of Fentanyl and Fentanyl Analogues from Whole Blood Using SPME Coupled to the Microfluidic Open Interface
Analytical Chemistry ( IF 6.7 ) Pub Date : 2023-12-29 , DOI: 10.1021/acs.analchem.3c04354 Emir Nazdrajić 1 , Daniel A Rickert 1 , Janusz Pawliszyn 1
Analytical Chemistry ( IF 6.7 ) Pub Date : 2023-12-29 , DOI: 10.1021/acs.analchem.3c04354 Emir Nazdrajić 1 , Daniel A Rickert 1 , Janusz Pawliszyn 1
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Fentanyl and its analogues are potent opioids that pose a significant threat to society. Over the last several years, considerable focus has been on the concerning trend of increasing fentanyl usage among drug users. Fentanyl analogues are mainly synthesized to evade analytical detection or increase their potency; thus, very low concentrations are sufficient to achieve a therapeutic effect. In an effort to help combat the synthetic opioid epidemic, developing targeted mass spectrometric methods for quantifying fentanyl and its analogues at ultralow concentrations is incredibly important. Most methods used to analyze fentanyl and its analogues from whole blood require manual sample preparation protocols (solid-phase extraction or liquid–liquid extraction), followed by chromatographic separation and mass spectrometric detection. The main disadvantages of these methods are the tedious sample preparation workflows, resulting in lengthy analysis times. To mitigate these issues, we present a targeted method capable of analyzing 96 samples containing fentanyl, several fentanyl analogues, and a common fentanyl (analogue) precursor simultaneously in 2.4 min per sample. This is possible by using a high-throughput solid phase microextraction workflow on the Concept96 autosampler followed by manual coupling of solid-phase microextraction fibers to the microfluidic open interface for tandem mass spectrometry analysis. Our quantitative method is capable of extremely sensitive analysis, with limits of quantification ranging from 0.002 to 0.031 ng mL–1 and linearity ranging from 0.010 to 25.0 ng mL–1. The method shows very good reproducibility (1–18%), accuracy (81–100%) of calibration and validation points, and good interday reproducibility (6–15%).
中文翻译：
使用与微流体开放接口耦合的 SPME 快速分析全血中的芬太尼和芬太尼类似物
芬太尼及其类似物是强效阿片类药物，对社会构成重大威胁。在过去的几年里，吸毒者中芬太尼使用量增加的趋势一直受到人们的广泛关注。芬太尼类似物的合成主要是为了逃避分析检测或增加其效力；因此，非常低的浓度就足以达到治疗效果。为了帮助对抗合成阿片类药物的流行，开发有针对性的质谱方法来定量超低浓度的芬太尼及其类似物非常重要。大多数用于分析全血中芬太尼及其类似物的方法都需要手动样品制备方案（固相萃取或液-液萃取），然后进行色谱分离和质谱检测。这些方法的主要缺点是繁琐的样品制备工作流程，导致分析时间过长。为了缓解这些问题，我们提出了一种有针对性的方法，能够在每个样品 2.4 分钟内同时分析 96 个含有芬太尼、几种芬太尼类似物和常见芬太尼（类似物）前体的样品。这可以通过在 Concept96 自动进样器上使用高通量固相微萃取工作流程，然后将固相微萃取纤维手动耦合到微流体开放接口进行串联质谱分析来实现。我们的定量方法能够进行极其灵敏的分析，定量限范围为 0.002 至 0.031 ng mL –1 ，线性范围为 0.010 至 25.0 ng mL –1 。该方法显示出非常好的校准和验证点再现性 (1–18%)、准确性 (81–100%) 以及良好的日间再现性 (6–15%)。
更新日期：2023-12-29
中文翻译：
使用与微流体开放接口耦合的 SPME 快速分析全血中的芬太尼和芬太尼类似物
芬太尼及其类似物是强效阿片类药物，对社会构成重大威胁。在过去的几年里，吸毒者中芬太尼使用量增加的趋势一直受到人们的广泛关注。芬太尼类似物的合成主要是为了逃避分析检测或增加其效力；因此，非常低的浓度就足以达到治疗效果。为了帮助对抗合成阿片类药物的流行，开发有针对性的质谱方法来定量超低浓度的芬太尼及其类似物非常重要。大多数用于分析全血中芬太尼及其类似物的方法都需要手动样品制备方案（固相萃取或液-液萃取），然后进行色谱分离和质谱检测。这些方法的主要缺点是繁琐的样品制备工作流程，导致分析时间过长。为了缓解这些问题，我们提出了一种有针对性的方法，能够在每个样品 2.4 分钟内同时分析 96 个含有芬太尼、几种芬太尼类似物和常见芬太尼（类似物）前体的样品。这可以通过在 Concept96 自动进样器上使用高通量固相微萃取工作流程，然后将固相微萃取纤维手动耦合到微流体开放接口进行串联质谱分析来实现。我们的定量方法能够进行极其灵敏的分析，定量限范围为 0.002 至 0.031 ng mL –1 ，线性范围为 0.010 至 25.0 ng mL –1 。该方法显示出非常好的校准和验证点再现性 (1–18%)、准确性 (81–100%) 以及良好的日间再现性 (6–15%)。
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