应用液相色谱/电喷雾串联质谱和液相色谱/四极杆飞行时间质谱同时检测各种基质中新精神活性物质的筛选方法。

Application of a simultaneous screening method for the detection of new psychoactive substances in various matrix samples using liquid chromatography/electrospray ionization tandem mass spectrometry and liquid chromatography/quadrupole time-of-flight mass spectrometry.

机构信息

Center for Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong Health Technology Administration Complex, 187 Osongsaengmyeong2-ro, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.

出版信息

Rapid Commun Mass Spectrom. 2021 May 30;35(10):e9067. doi: 10.1002/rcm.9067.

DOI:10.1002/rcm.9067

PMID:33656207

Abstract

RATIONALE

Recently, new psychoactive substances (NPS) have emerged as a public health risk. Particularly, their chemical structures are modified to avoid detection. Synthetic NPS with effects similar to those of illegal drugs have been recently detected and synthesized worldwide, including MDMB-FUBINACA and APINAC, making it essential to rapidly and accurately detect NPS.

METHODS

Fourteen NPS with similar structures were selected and their structures identified using H and C NMR spectroscopy. Additionally, we proposed the fragmentation pattern of each compound using liquid chromatography/quadrupole time-of-flight mass spectrometry (LC/QTOF-MS). A simultaneous analytical method using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) was also developed and applied to real samples to detect the 14 NPS. The method was validated based on the specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, matrix effect, and stability according to international validation guidelines.

RESULTS

The established method was used to screen 65 different matrix samples using LC/ESI-MS/MS. By comparing the calculated product ion ratios with those of standards, 2C-B in one of the real samples and 5F-MDMB-PICA in 20 samples were identified. For re-confirmation of detected compounds, the fragmentation pattern of each compound was compared with that of each standard using LC/QTOF-MS.

CONCLUSIONS

In this study, LC/QTOF-MS data were used to elucidate the structures and fragmentation patterns of 14 NPS. A simultaneous method was developed using LC/ESI-MS/MS, which was applied to 65 real samples. The presented method and results can assist in ensuring the safety of public health from illegal adulteration.

摘要

原理

最近，新精神活性物质（NPS）已成为公共健康风险。特别是，它们的化学结构经过修饰以避免被检测到。具有类似非法药物作用的合成 NPS 已在全球范围内被最近检测和合成，包括 MDMB-FUBINACA 和 APINAC，因此必须快速准确地检测 NPS。

方法

选择了 14 种结构相似的 NPS，并使用 H 和 C NMR 光谱鉴定其结构。此外，我们还使用液相色谱/四极杆飞行时间质谱（LC/QTOF-MS）提出了每种化合物的断裂模式。还开发并应用了一种同时使用液相色谱/电喷雾串联质谱（LC/ESI-MS/MS）的分析方法来检测 14 种 NPS。该方法根据国际验证指南，基于特异性、线性、检测限（LOD）、定量限（LOQ）、精密度、准确度、基质效应和稳定性进行了验证。

结果

使用 LC/ESI-MS/MS 对 65 种不同基质样品进行了筛选。通过将计算出的产物离子比与标准品进行比较，在其中一个实际样品中鉴定出了 2C-B，在 20 个样品中鉴定出了 5F-MDMB-PICA。为了对检测到的化合物进行重新确认，使用 LC/QTOF-MS 比较了每种化合物的断裂模式与每种标准品的断裂模式。