Analyzing fentanyl and fentanyl analogues by ion mobility spectrometry

Zaknoun, Hafid; Binette, Marie-Josée; Tam, Maggie

doi:10.1007/s12127-019-00244-0

Cited by 37 publications

(33 citation statements)

References 8 publications

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“…Due to their high sensitivity, fast response times, and compact design, ion mobility spectrometers are commonly used in safety and security applications such as the detection of chemical warfare agents, 1,2 toxic industrial chemicals, 3,4 drugs, 5,6 and explosives 7–9 . Basically, ion mobility spectrometry (IMS) instruments can be divided by their principle of ion separation.…”

Section: Introductionmentioning

confidence: 99%

Formation of positive product ions from substances with low proton affinity in high kinetic energy ion mobility spectrometry

Allers

Kirk

Schaefer

et al. 2021

Rapid Comm Mass Spectrometry

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Rationale: Ion mobility spectrometry (IMS) instruments are typically equipped with atmospheric pressure chemical ionization (APCI) sources operated at ambient pressure. However, classical APCI-IMS suffers from a limited ionization yield for nonpolar substances with low proton affinity (PA). This is mainly due to ion clustering processes, especially those that involve water molecules, inhibiting the ionization of these substances. Methods: High Kinetic Energy (HiKE)-IMS instruments are operated at decreased pressures and high reduced electric field strengths. As most clustering reactions are inhibited under these conditions, the ionization yield for nonpolar substances with low PA in HiKE-IMS should differ from that in classical APCI-IMS. To gain first insights into the ionization capabilities and limitations of HiKE-IMS, we investigated the ionization of four model substances with low PA in HiKE-IMS using HiKE-IMS-MS as a function of the reduced electric field strength. Results: The four model substances all have proton affinities between those of H 2 O and (H 2 O) 2 but exhibit different ionization energies, dipole moments, and polarizabilities. As expected, the results show that the ionization yield for these substances differs considerably at low reduced electric field strengths due to ion cluster formation. In contrast, at high reduced electric field strengths, all substances can be ionized via charge and/or proton transfer in HiKE-IMS. Conclusions: Considering the detection of polar substances with high PAs, classical ambient pressure IMS should reach better detection limits than HiKE-IMS. However, considering the detection of nonpolar substances with low PA that are not detected, or only difficult to detect, at ambient pressure, HiKE-IMS would be beneficial. 1 | INTRODUCTION Due to their high sensitivity, fast response times, and compact design, ion mobility spectrometers are commonly used in safety and security applications such as the detection of chemical warfare agents, 1,2 toxic industrial chemicals, 3,4 drugs, 5,6 and explosives. 7-9 Basically, ion mobility spectrometry (IMS) instruments can be divided by their principle of ion separation. In this work, a drift tube (DT) ion mobility spectrometer is used. In DT-IMS, ions are separated by their motion along the axis of a drift tube driven by a homogeneous static electric field. To initiate the measurement, an ion packet is injected into the drift tube. During their motion, the ions are separated based on the absolute value of their ion mobility in the present drift gas. At the end of the drift tube, the ions are captured by a detector that converts

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Section: Introductionmentioning

confidence: 99%

Formation of positive product ions from substances with low proton affinity in high kinetic energy ion mobility spectrometry

Allers

Kirk

Schaefer

et al. 2021

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

show abstract

“…Alternatively, IMS can suffer from competitive ionization between fentanyl and excipients present in drug mixtures (e.g., procaine), as well as exhibit difficulties resolving heroin and fentanyl, creating challenges for analysis of complex drug mixtures. 12,13 Extensive work has been reported for the detection of fentanyl using several liquid chromatography mass spectrometry (LC-MS) based techniques. [14][15][16][17][18][19][20] LC-MS/MS for the detection of 16 opioids, fentanyl, and 8 fentanyl analogues in both blood and urine from ten autopsy samples 16 whereas Elbardisy, et al circumvented MS by applying high-performance liquid chromatography (HPLC) with diode array detection and HPLC with amperometry detection for analysis of heroin, fentanyl, and 10 fentanyl analogues 21 .…”

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confidence: 99%

Separation and Detection of Trace Fentanyl from Complex Mixtures Using Gradient Elution Moving Boundary Electrophoresis

2019

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The current opioid epidemic remains an ongoing challenge, exacerbated by the extreme potency of synthetic opioids (e.g., fentanyl and fentanyl analogues), leading to an increase in adulterated heroin-related deaths. The increasing prevalence of fentanyl and fentanyl analogues in mixtures with heroin and other adulterants, excipients, and bulking agents has placed an emphasis on trace analysis methods for their detection from complex drug mixtures. Here, gradient elution moving boundary electrophoresis (GEMBE), a robust and miniaturized electrophoretic separation technique, was employed for the separation and detection of fentanyl and nine (9) fentanyl analogues from mixtures. GEMBE incorporated a short capillary (5 cm × 15 μm i.d.) for the electrophoretic separation of analytes with an opposing bulk counterflow. As the velocity of the counterflow was varied, analytes with differing electrophoretic mobilities entered the separation channel at different times and were analyzed as moving boundaries by contactless conductivity detection. The continuous injection of sample, driven by a controlled and variable pressure, both provided selectivity of the analytes and prevented contaminants or particulate within the sample from entering the separation capillary. Fentanyl was successfully separated and detected down to 2.5 μmol/L, and demonstrated only 50 % to 60 % signal suppression in dilute binary mixtures with heroin and other common adulterants and excipients at 30:1 (compound:fentanyl) concentration ratios. In addition, GEMBE was successfully applied to a few adjudicated case samples of fentanyl-related mixtures exhibiting dyes and visible particulate. The short capillaries, contactless detection format utilized here, and continuous injection of sample allows for a small footprint platform that is easy-to-use for forensic analyses.

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“…Besides, by compressing the ion packet twice during the injection process, the dual-compression tristate ion shutter mode surpassed the other two shutter modes in sensitivity for sufentanil, which also enhanced the observation of the dimer ion and hence contributed to the accurate identification of sufentanil. Notably, none of the previous studies relating to the IMS-analysis of fentanyl or its analogues has reported any dimer peak. − …”

Section: Resultsmentioning

confidence: 99%

Miniaturized Ion Mobility Spectrometer with a Dual-Compression Tristate Ion Shutter for On-Site Rapid Screening of Fentanyl Drug Mixtures

Chen

Huang

et al. 2019

Anal. Chem.

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The hidden presence of fentanyl and new psychoactive substances in established illicit drugs has led to a great number of unintentional fatal overdoses, justifying the urgent need for portable tools for the rapid screening of various drugs. Ion mobility spectrometry, as a rapid detection technique, has been widely used in detecting illicit drugs, whereas it is insufficiently sensitive for bigger ions due to the mobility discrimination of an ion shutter. In this work, a miniaturized ion mobility spectrometer with an inner diameter of 14 mm and a drift length of 38.9 mm and equipped with a novel dual-compression tristate ion shutter has been developed, which could greatly reduce the mobility discrimination by compressing the ion packet twice during the injection process. The best gating performance of the dualcompression tristate ion shutter was about three times as high as that of the tristate ion shutter and twice as high as that of the Tyndall-Powell shutter. For example, the peak height was increased by 150 or 40% when the resolving power was the same, whereas the resolution of two neighboring peaks was improved by 46 or 19% when the peak heights were the same. In screening of fentanyl drug mixtures, the new shutter enhanced the identification accuracy of constituents by making peaks of slow dimer ions and complex ions observable. Besides, the new shutter helped to achieve high sensitivity for drug ions spreading a wide ion mobility range from 0.644 to 2.032 cm 2 s −1 V −1 , demonstrating its potential use in the analysis of other mixtures and the detection of large ions.

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Analyzing fentanyl and fentanyl analogues by ion mobility spectrometry

Cited by 37 publications

References 8 publications

Formation of positive product ions from substances with low proton affinity in high kinetic energy ion mobility spectrometry

Formation of positive product ions from substances with low proton affinity in high kinetic energy ion mobility spectrometry

Separation and Detection of Trace Fentanyl from Complex Mixtures Using Gradient Elution Moving Boundary Electrophoresis

Miniaturized Ion Mobility Spectrometer with a Dual-Compression Tristate Ion Shutter for On-Site Rapid Screening of Fentanyl Drug Mixtures

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