US Drug Enforcement Administration, 22624 Dulles Summit Court, Dulles, VA 20166, USA.
US Drug Enforcement Administration, 22624 Dulles Summit Court, Dulles, VA 20166, USA.
Forensic Sci Int. 2021 Jan;318:110565. doi: 10.1016/j.forsciint.2020.110565. Epub 2020 Nov 1.
With the recent development of hand-held and miniature mass spectrometers, low cost and compact mass detectors have become more available and accessible for on-site and routine laboratory use. Here we present a rapid ultra-high performance liquid chromatography-photodiode array/mass spectrometry (UHPLC-PDA/MS) method for the routine screening of a wide variety of illicit drugs using a small and cost effective single quadrupole MS (SQD) with electron spray ionization (ESI). Two libraries for common drugs of forensic interest, a PDA library including retention time (RT) and PDA spectra and a MS library including RT and [M+H]/[M-H], were developed. Using a BEH phenyl column and gradient elution of acetonitrile and 0.1% formic acid, drugs of forensic interest were detected within 8.5min and identified based on their RT/RRT to an internal standard (Codeine-d), UV spectrum, and/or MS spectrum/(de)protonated molecular mass. The method proved to be efficient, reproducible, and sensitive with a limit of detection (LOD) ≤0.5μg/mL for untargeted screening using PDA and MS in full scan mode and ≤0.1μg/mL for targeted screening by MS in select ion recording (SIR) mode. Improved isomer discrimination was achieved, when a second injection and separation by a charged column (CSH C) was incorporated into the same acquisition sequence. The method was applied to 20 seized drugs with similar detection limits and identifications by GC-MS. Using an orthogonal separation technique and dual detection systems, the UHPLC-PDA/SQD method serves as an attractive technique for a direct and fast screening of illicit drugs with excellent discrimination power and detection capacity. The developed method can be an alternative screening method to GC-FID and complementary technique to GC-MS for routine forensic drug screening.
随着手持式和微型质谱仪的最新发展，低成本和紧凑型质量检测器变得更加普及和适用于现场和常规实验室使用。在这里，我们提出了一种快速的超高效液相色谱-光电二极管阵列/质谱（UHPLC-PDA/MS）方法，用于使用具有电子喷雾电离（ESI）的小型且经济高效的单四极杆 MS（SQD）对各种非法药物进行常规筛选。为了共同的法医学感兴趣的药物，我们开发了一个 PDA 库，包括保留时间（RT）和 PDA 光谱，以及一个 MS 库，包括 RT 和 [M+H]/[M-H]，包括两个库。使用 BEH 苯基柱和乙腈和 0.1%甲酸的梯度洗脱，在 8.5 分钟内检测到法医学感兴趣的药物，并根据其相对于内标（可待因-d）、紫外光谱和/或 MS 光谱/去质子化分子质量的 RT/RRT 进行鉴定。该方法被证明是高效、可重现且灵敏的，使用 PDA 和 MS 全扫描模式进行非靶向筛选的检测限（LOD）≤0.5μg/mL，MS 在选择离子记录（SIR）模式下进行靶向筛选的检测限≤0.1μg/mL。当将第二次注射和分离通过带电柱（CSH C）纳入相同的采集序列时，可以实现更好的异构体鉴别。该方法应用于 20 种缴获的药物，其 GC-MS 检测限和鉴定结果相似。使用正交分离技术和双检测系统，UHPLC-PDA/SQD 方法是一种有吸引力的技术，可用于直接快速筛选非法药物，具有出色的鉴别力和检测能力。该方法可以作为 GC-FID 的替代筛选方法，也是 GC-MS 进行常规法医药物筛选的补充技术。
