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An ultra-rapid drug screening method for acetaminophen in blood serum based on probe electrospray ionization-tandem mass spectrometry
Journal of Food and Drug Analysis ( IF 2.6 ) Pub Date : 2019-07-01 , DOI: 10.1016/j.jfda.2019.02.001 Kiyotaka Usui 1 , Haruka Kobayashi 1 , Yuji Fujita 2 , Eito Kubota 1 , Tomoki Hanazawa 3 , Tomohiro Yoshizawa 3 , Yoshito Kamijo 3 , Masato Funayama 1
Journal of Food and Drug Analysis ( IF 2.6 ) Pub Date : 2019-07-01 , DOI: 10.1016/j.jfda.2019.02.001 Kiyotaka Usui 1 , Haruka Kobayashi 1 , Yuji Fujita 2 , Eito Kubota 1 , Tomoki Hanazawa 3 , Tomohiro Yoshizawa 3 , Yoshito Kamijo 3 , Masato Funayama 1
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Poisoning incidents caused by drugs, accidental ingestion of poisons, attempted suicide, homicide, and exposure to toxic compounds occur frequently every year across the globe. This raises the need to rapidly identify toxic agents in poisoned patients in a clinical emergency setting. In addition, determining drug/poison concentration is undoubtedly necessary to arrive at a toxicological treatment plan. The purpose of this study was to develop an ultra-rapid drug screening method for the clinical treatment of poisoning. Probe electrospray ionization (PESI), one of the ambient ionization techniques, is able to detect compounds from various biological materials almost directly. We applied the PESI technique to the rapid detection of acetaminophen (APAP). Blood serum samples were diluted 100-fold with 10 mM ammonium formate/ethanol (1:1 v/v) solution including deuterium-labeled internal standards (IS; APAP-d4). Only 10 μL of the diluted sample was used for measurement. The tandem mass spectrometer (MS/MS) equipped with a PESI was used in selected reaction monitoring mode for the quantitation of APAP; the measurement time was only 18 s. Transitions were set at 152 > 110 for quantitation, 152 > 65 for qualifier, and 156 > 114 for IS (APAP-d4). All measurements were conducted in positive mode. The calibration curve (1/x2) was linear over the range of 1.56-200 μg/mL (r2 = 0.998), and the limit of detection and quantitation were 0.37 μg/mL and 1.56 μg/mL, respectively. The accuracy (bias) and precision (RSD%) of the method were within an acceptable range (-0.15-2.8% and 2.3-6.1%, respectively) and matrix effect at 3 concentrations (95.1-104%) indicated that PESI-MS/MS is only slightly affected by matrices. In real forensic cases, quantitative values of APAP determined by the PESI-MS/MS were almost identical to those determined by the liquid chromatography-MS/MS method. Since PESI-MS/MS is a simple, reliable, and rapid determination method for toxic agents with virtually no need for blood serum pre-treatment, it would be highly suitable for poisoning cases in clinical emergency settings. In the future, a method for simultaneous rapid determination of multiple toxic agents will be developed.
中文翻译：
基于探针电喷雾电离-串联质谱法的血清中对乙酰氨基酚药物超快速筛查方法
全球每年因毒品、误食毒物、自杀未遂、杀人、接触有毒化合物等引起的中毒事件时有发生。这就提出了在临床紧急情况下快速识别中毒患者体内有毒物质的需求。此外，确定药物/毒物浓度对于制定毒理学治疗计划无疑是必要的。本研究的目的是开发一种用于临床治疗中毒的超快速药物筛选方法。探针电喷雾电离 (PESI) 是环境电离技术之一，能够几乎直接检测各种生物材料中的化合物。我们将 PESI 技术应用于对乙酰氨基酚 (APAP) 的快速检测。用 10 mM 甲酸铵/乙醇 (1:1 v/v) 溶液（包括氘标记的内标物（IS；APAP-d4））将血清样品稀释 100 倍。仅使用 10 μL 稀释样品进行测量。配备 PESI 的串联质谱仪 (MS/MS) 在选定的反应监测模式下用于 APAP 的定量；测量时间仅为18秒。定量的离子对设置为 152 > 110，定性离子的离子对设置为 152 > 65，IS (APAP-d4) 的离子对设置为 156 > 114。所有测量均在正模式下进行。校准曲线(1/x2)在1.56-200 μg/mL范围内呈线性(r2 = 0.998)，检测限和定量限分别为0.37 μg/mL和1.56 μg/mL。该方法的准确度（偏倚）和精密度（RSD%）均在可接受的范围内（分别为-0.15-2.8%和2.3-6.1%），并且3个浓度（95.1-104%）的基质效应表明PESI-MS /MS 仅受矩阵轻微影响。 在真实的法医案件中，PESI-MS/MS 测定的 APAP 定量值与液相色谱-MS/MS 法测定的 APAP 定量值几乎相同。由于PESI-MS/MS是一种简单、可靠、快速的有毒物质测定方法，几乎不需要血清预处理，因此非常适合临床紧急情况下的中毒病例。未来将开发一种同时快速测定多种有毒物质的方法。
更新日期：2019-07-01
中文翻译：
基于探针电喷雾电离-串联质谱法的血清中对乙酰氨基酚药物超快速筛查方法
全球每年因毒品、误食毒物、自杀未遂、杀人、接触有毒化合物等引起的中毒事件时有发生。这就提出了在临床紧急情况下快速识别中毒患者体内有毒物质的需求。此外，确定药物/毒物浓度对于制定毒理学治疗计划无疑是必要的。本研究的目的是开发一种用于临床治疗中毒的超快速药物筛选方法。探针电喷雾电离 (PESI) 是环境电离技术之一，能够几乎直接检测各种生物材料中的化合物。我们将 PESI 技术应用于对乙酰氨基酚 (APAP) 的快速检测。用 10 mM 甲酸铵/乙醇 (1:1 v/v) 溶液（包括氘标记的内标物（IS；APAP-d4））将血清样品稀释 100 倍。仅使用 10 μL 稀释样品进行测量。配备 PESI 的串联质谱仪 (MS/MS) 在选定的反应监测模式下用于 APAP 的定量；测量时间仅为18秒。定量的离子对设置为 152 > 110，定性离子的离子对设置为 152 > 65，IS (APAP-d4) 的离子对设置为 156 > 114。所有测量均在正模式下进行。校准曲线(1/x2)在1.56-200 μg/mL范围内呈线性(r2 = 0.998)，检测限和定量限分别为0.37 μg/mL和1.56 μg/mL。该方法的准确度（偏倚）和精密度（RSD%）均在可接受的范围内（分别为-0.15-2.8%和2.3-6.1%），并且3个浓度（95.1-104%）的基质效应表明PESI-MS /MS 仅受矩阵轻微影响。 在真实的法医案件中，PESI-MS/MS 测定的 APAP 定量值与液相色谱-MS/MS 法测定的 APAP 定量值几乎相同。由于PESI-MS/MS是一种简单、可靠、快速的有毒物质测定方法，几乎不需要血清预处理，因此非常适合临床紧急情况下的中毒病例。未来将开发一种同时快速测定多种有毒物质的方法。
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