Validated method for the analysis of 22 illicit drugs and their metabolites via liquid chromatography tandem mass spectrometry (LC-MS/MS) in illicit drug samples collected in Chicago, IL

Whitehead, Heather D.; Hayes, Kathleen L.; Swartz, James A.; Prete, Elizabeth; Robison-Taylor, Lisa; Mackesy‐Amiti, Mary Ellen; Jimenez, Antonio D.; Lieberman, Marya

doi:10.1016/j.forc.2023.100475

Cited by 14 publications

(12 citation statements)

References 32 publications

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“…This nding is in-line with previous reports of the LOD of BTNX strips, which found the working limit of detection for drug checking to be between 100-200 ng/mL. [13][14][15][16][17] There are no literature reports of the limit of detection for DanceSafe FTS for drug checking applications.…”

Section: Comparison Of Btnx and Dancesafe Fts Resultssupporting

confidence: 86%

“…These reports cite incidence of false positives between 0-9.6% and false negatives between 3.7-10.9%, and limits of detection between 100-200 ng/mL. [13][14][15][16][17] Cross-reactivity of FTS with methamphetamine, MDMA, and diphenhydramine-a common cutting agent in illicit drugs-is a major drawback of BTNX Rapid Response FTS but ultimately researchers have concluded that FTS are a valid and useful tool for drug checking. [13,18] In part due to the relatively large amount of research on the product, BTNX Rapid Response FTS have been the major brand adopted by harm reduction organizations for drug checking.…”

Section: Introductionmentioning

confidence: 99%

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Assessment of two brands of fentanyl test strips with 251 synthetic opioids reveals “blind spots” in detection capabilities

Hayes,

Lieberman

2023

Preprint

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Background Fentanyl test strips (FTS) are a commonly deployed tool in drug checking, used to test for the presence of fentanyl in street drug samples prior to consumption. Previous reports indicate that in addition to fentanyl, FTS can also detect potent fentanyl analogs like acetyl fentanyl and butyryl fentanyl, with conflicting reports on their ability to detect prominent fentanyl analogs like carfentanil and furanyl fentanyl. Yet with hundreds of known fentanyl analogs, there has been no large-scale study rationalizing FTS reactivity to different fentanyl analogs. Methods In this study, 251 synthetic opioids- including 214 fentanyl analogs- were screened on two brands of fentanyl test strips to 1) assess the differences in the ability of two brands of fentanyl test strips to detect fentanyl-related compounds and 2) determine which moieties in fentanyl analog chemical structures are most crucial for FTS detection. Two FTS brands were assessed in this study: BTNX Rapid Response and WHPM DanceSafe. Results Of 251 screened compounds assessed, 121 compounds were detectable at or below 20,000 ng/mL by both BTNX and DanceSafe FTS, 50 were not detectable by either brand, and 80 were detectable by one brand but not the other (n = 52 BTNX, n = 28 DanceSafe). A structural analysis of fentanyl analogs screened revealed that in general bulky modifications to the phenethyl moiety inhibit detection by BTNX FTS while bulky modifications to the carbonyl moiety inhibit detection by DanceSafe FTS; we hypothesize that the different “blind spots” may be caused by different haptens used to elicit the antibodies for these different strips. Conclusions By utilizing both brands of FTS in routine drug checking, users could increase the chances of detecting fentanyl analogs in the “blind spot” of one brand.

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Section: Comparison Of Btnx and Dancesafe Fts Resultssupporting

confidence: 86%

Section: Introductionmentioning

confidence: 99%

Assessment of two brands of fentanyl test strips with 251 synthetic opioids reveals “blind spots” in detection capabilities

Hayes,

Lieberman

2023

Preprint

Self Cite

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“…These findings indicated a slightly higher LOD in comparison with results obtained using triple quadrupole‐based MS/MS, which have shown LODs ranging from 3–7 pg/mL 67,68 . However, the quantitative performance of our study is still higher than the findings of Whitehead et al, 69 who reported an LOD of 23.8 pg/mL and an LOQ of 0.1 ng/mL for fentanyl. In triplicate runs, the concentration of 100 ng/mL yielded an average percent recovery of 86% and a matrix effect of 10%.…”

Section: Resultscontrasting

confidence: 84%

Improved separation of fentanyl isomers using metal cation adducts and high‐resolution ion mobility‐mass spectrometry

Aderorho,

Chouinard

2023

Drug Testing and Analysis

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Fentanyl is a potent synthetic opioid that has attracted significant attention due to its illegal production and distribution, resulting in misuse, overdose, and fatalities. Because numerous fentanyl analogs, including structural isomers, with different potency have been discovered in the field, there is a critical need to continue developing analytical methodologies capable of accurate identification in forensic and clinical laboratories. This study aimed to develop a rapid method for detecting and separating fentanyl isomers based on ion mobility–mass spectrometry (IM‐MS), where IM separates gas‐phase ions based on differences in their size, shape, and charge. Several strategies for improved differentiation were implemented, including using unconventional cation adducts (e.g., alkali and transition metals) and data post‐processing by high‐resolution demultiplexing. A collection of collision cross section (CCS) values for the various metal ion adducts was gathered, which can be used to improve confidence of identification in future samples. Notable examples, such as [M + Cu]+ and [M + Ag]+ adducts, contributed to significant improvement of resolution between isomers. Furthermore, the addition of high‐resolution post‐processing provided resolving power of >150, which constitutes a significant increase in comparison with the normal 50–60 obtained with low‐resolution drift tube instruments. Collectively, these improved separation strategies allowed for confident detection and subsequent quantitative analysis. The optimized IM‐MS method resulted in quantification of fentanyl in human urine with limits of detection and quantification of 13 pg/mL and 40 pg/mL, respectively.

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“…In the context of increasingly complex substances and unprecedented levels of illicit drug overdose, there are significant advantages to a multi-instrument approach to drug checking [ 31 , 33 , 123 ]. Using more than one method for drug identification has advantages in terms of increased confidence when a particular component is detected by more than one technique, and increased awareness when something is detected by at least but perhaps only one technique.…”

Section: Discussionmentioning

confidence: 99%

Point-of-care community drug checking technologies: an insider look at the scientific principles and practical considerations

2023

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Drug checking is increasingly being explored outside of festivals and events to be an ongoing service within communities, frequently integrated within responses to illicit drug overdose. The choice of instrumentation is a common question, and the demands on these chemical analytical instruments can be challenging as illicit substances may be more complex and include highly potent ingredients at trace levels. The answer remains nuanced as the instruments themselves are not directly comparable nor are the local demands on the service, meaning implementation factors heavily influence the assessment and effectiveness of instruments. In this perspective, we provide a technical but accessible introduction to the background of a few common drug checking methods aimed at current and potential drug checking service providers. We discuss the following tools that have been used as part of the Vancouver Island Drug Checking Project in Victoria, Canada: immunoassay test strips, attenuated total reflection IR-absorption spectroscopy, Raman spectroscopy from powder samples, surface-enhanced Raman scattering in a solution of colloidal gold nanoparticles, and gas chromatography–mass spectrometry. Using four different drug mixtures received and tested at the service, we illustrate the strengths, limitations, and capabilities of such instruments, and expose the scientific theory to give further insight into their analytical results. Each case study provides a walk-through-style analysis for a practical comparison between data from several different instruments acquired on the same sample. Ideally, a single instrument would be able to achieve all of the objectives of drug checking. However, there is no clear instrument that ticks every box; low cost, portable, rapid, easy-to-use and provides highly sensitive identification and accurate quantification. Multi-instrument approaches to drug checking may be required to effectively respond to increasingly complex and highly potent substances demanding trace level detection and the potential for quantification.

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Validated method for the analysis of 22 illicit drugs and their metabolites via liquid chromatography tandem mass spectrometry (LC-MS/MS) in illicit drug samples collected in Chicago, IL

Cited by 14 publications

References 32 publications

Assessment of two brands of fentanyl test strips with 251 synthetic opioids reveals “blind spots” in detection capabilities

Assessment of two brands of fentanyl test strips with 251 synthetic opioids reveals “blind spots” in detection capabilities

Improved separation of fentanyl isomers using metal cation adducts and high‐resolution ion mobility‐mass spectrometry

Point-of-care community drug checking technologies: an insider look at the scientific principles and practical considerations

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