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通过 96 孔固相微萃取传输模式和实时直接分析质谱法对生物流体中的滥用药物进行高通量定量分析。

High-throughput quantification of drugs of abuse in biofluids via 96-solid-phase microextraction-transmission mode and direct analysis in real time mass spectrometry.

机构信息

Department of Chemistry, University of Waterloo, Ontario, N2L 3G1, Canada.

Restek Corporation, Bellefonte, Pennsylvania, 16823, USA.

出版信息

Rapid Commun Mass Spectrom. 2019 Sep 30;33(18):1423-1433. doi: 10.1002/rcm.8477.

Abstract

RATIONALE

The workload of clinical laboratories has been steadily increasing over the last few years. High-throughput (HT) sample processing allows scientists to spend more time undertaking matters of critical thinking rather than laborious sample processing. Herein we introduce a HT 96-solid-phase microextraction (SPME) transmission mode (TM) system coupled to direct analysis in real time (DART) mass spectrometry (MS).

METHODS

Model compounds (opioids) were extracted from urine and plasma samples using a 96-SPME-TM device. A standard voltage and pressure (SVP) DART source was used for all experiments. Examination of SPME-TM performance was done using high-resolution mass spectrometry (HRMS) in full scan mode (100-500 m/z), whereas quantitation of opioids was performed using triple quadrupole MS in multiple reaction monitoring mode and by using a matrix-matched internal standard correction method.

RESULTS

Thirteen points (0.5 to 200 ng mL ) were used to establish a calibration curve. Low limits of quantitation (LOQ) were obtained (0.5 to 25 ng mL ) for matrices used. Acceptable accuracy (71.4-129.4%) and repeatability (1.1-24%) were obtained for validation levels tested (0.5, 30 and 90 ng mL ). In less than 1.5 hours, 96 samples were extracted, desorbed and processed using the 96-SPME-TM system coupled to DART-MS.

CONCLUSIONS

A rapid HT method for detection of opioids in urine and plasma samples was developed. This study demonstrated that ambient ionization mass spectrometry coupled to robust sample preparation methods such as SPME-TM can rapidly and efficiently screen/quantify target analytes in a HT context.

摘要

原理

近年来,临床实验室的工作量一直在稳步增加。高通量(HT)样品处理可让科学家有更多时间进行批判性思维的事项,而不是繁琐的样品处理。在此,我们介绍一种 HT 96-固相微萃取(SPME)传输模式(TM)系统,该系统与实时直接分析(DART)质谱(MS)相结合。

方法

使用 96-SPME-TM 设备从尿液和血浆样品中提取模型化合物(阿片类药物)。所有实验均使用标准电压和压力(SVP)DART 源。使用高分辨率质谱(HRMS)在全扫描模式(100-500 m/z)下检查 SPME-TM 的性能,而使用三重四极杆 MS 在多重反应监测模式下定量阿片类药物,并使用基质匹配的内标校正方法。

结果

使用 13 个点(0.5 至 200 ng·mL )建立校准曲线。在所使用的基质中,获得了低定量下限(LOQ)(0.5 至 25 ng·mL )。在测试的验证水平(0.5、30 和 90 ng·mL )上,获得了可接受的准确度(71.4-129.4%)和重复性(1.1-24%)。使用 96-SPME-TM 系统结合 DART-MS,在不到 1.5 小时的时间内即可提取、解吸和处理 96 个样品。

结论

开发了一种用于尿液和血浆样品中阿片类药物检测的快速 HT 方法。本研究表明,大气压电离质谱与 SPME-TM 等强大的样品制备方法相结合,可以在 HT 环境中快速有效地筛选/定量目标分析物。

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