Utilizing coiled microextraction and portable GC/MS for fentanyl analogs rapid in-field screening

Recent years have seen a notable increase in fatalities related to the use and consumption of opioids - a class of synthetically manufactured pain-relieving drugs that are similar to naturally derived opiates; for example, opium, morphine, codeine and heroin.

Opioids serve as fast-acting solutions to severe pain management when properly administered in appropriate dosages, prompting their inclusion on the World Health Organization’s List of Essential Medicines.1

Both opioid and opiate-type drugs possess a high-risk factor for physical dependence. This, coupled with the accompanying euphoric sensations that both opioid and opiate-type drugs offer, has prompted significant abuse and misuse on a global scale.

The United Nations World Drug Report issued in 2017 stated that opioids were responsible for considerable proportion of global fatalities and 70% of diseases acquired through drug use.2

The seriousness of this issue has become especially evident in the United States, where misuse of pharmaceutical opioids coupled with increased heroin and fentanyl use has led to the death rate tripling from 16,849 to 52,404 annually between 1999 and 2015.2

The misuse of prescription opioids and opiates is a major factor in this ongoing epidemic. The opioid market is becoming more diversified, leading to an increase in new drugs commonly known as new psychoactive substances (NPS).

Manufactured in clandestine laboratories around the globe, NPS has been discovered in counterfeit medicines design to appear identical to pharmaceutical products despite containing fentanyl analogs and other non-opioid substances.2

A range of counterfeit drugs and heroin seized following fatal overdoses were found to include fentanyl analogs. These analogs included acetyl fentanyl, 3-methylfentanyl and carfentanil – a highly potent opioid and veterinary painkiller utilized for large animals that is around 10,000 times as strong as morphine.3

Counterfeit pills and powders exhibit variations in potency and quantity of active components. This makes them a considerable threat to both users and first responders which may be exposed to the drugs at clandestine laboratories or intercepted via efforts to halt drug trafficking.

The sheer gravity of this opioid epidemic has created an intense need for an analytical solution that is able to safely screen confiscated drugs and samples from clandestine laboratories for the presence of fentanyl analogs.

Gas Chromatography-Mass Spectrometry (GC/MS) has been regarded as the gold standard for controlled substance identification for decades because GC/MS can facilitate the detection of a broad range of analytes in a diverse range of sample mixtures.

Samples prepared for GC/MS are generally collected on-site before being transported to a forensic laboratory for analysis. This process often takes months, however, due to current case backlogs and the prolonged analysis times of 15 to 60 minutes typically associated with conventional benchtop units.4,5

One alternative means of reducing the time between collection and analysis is to bring the laboratory to the sample through the utilization of portable GC/MS technology. Portable GC/MS technology used in conjunction with rapid sampling techniques is able to acquire actionable results fast.

This article explores the use of the novel Custodion® Coiled Microextraction (CME) syringes with the Torion® T-9 Portable GC/MS as a quick and user-friendly screening tool for both drugs of abuse and new psychoactive substances (NPS) in the field.

The examples presented here employ the Torion® T-9 Portable GC/MS in the screening of three opioids: fentanyl, acetyl fentanyl and carfentanil. These three opioids are frequently found in clandestine laboratories, as well as being used as cutting agents in counterfeit medications and heroin.

Data acquired via these analyses was matched against the Wiley Designer Drug Library via Chromion Software. This process took around 8 minutes from sample collection to identification.

Custodion® coiled microextraction

Coiled Microextraction (CME) is a novel sampling technique developed by PerkinElmer Inc. CME uses a single device to combine liquid sample collection and preparation, enabling the straightforward sampling of drugs of abuse or explosives in the field.

The coiled wire present within the Custodion-CME syringe is comprised of an inertium treated wire that has been finely coiled to capture liquid samples. The Custodian’s hardened plastic design handle is as simple to use as a retractable ball-point pen, allowing users to deploy the CME wire with a single button press.

The device’s modest design and its flexible blunt tip help avoid the safety concerns of a conventional sharp syringe. This means that users working with personal protective equipment (PPE) are still free to collect samples with one hand.

Custodion® Coiled Microextraction (CME) syringe with an extended coiled wire.

Figure 1. Custodion® Coiled Microextraction (CME) syringe with an extended coiled wire. Image Crdit: PerkinElmer

Torion® T-9 Portable GC/MS

The Torion® T-9 Portable GC/MS has been built for portability and rapid analysis, offering equivalent chromatographic performance to a benchtop system in a fraction of the time.

Torion® technology works by integrating a low thermal mass (LTM) capillary gas chromatograph with a miniaturized toroidal ion trap mass spectrometer. This results in the provision of a reliable, fast and easy-to-use GC/MS while also ensuring minimal power consumption in the field.

The Torion® T-9 Portable GC/MS has a total weight of 32 pounds (14.5 kg). The instrument also boasts a suite of versatile sample collection devices, allowing it to be deployed on-site to quickly screen a range of samples, for example:

  • Environmental volatiles and semi-volatiles (VOCs/SVOCs)
  • Drugs of abuse
  • Explosives
  • Chemical threats
  • Hazardous substances

Experimental and sample preparation

Analytical grade standards of fentanyl, acetyl fentanyl, carfentanil and heroin were acquired from Cerilliant Corp. (Round Rock, TX, USA). These were all provided at 1.0 mg/mL concentrations.

Mock clandestine laboratory samples of fentanyl, acetyl fentanyl and carfentanil were synthesized at the University of North Texas (Denton, TX, USA).

A Custodion-CME syringe was utilized for sample collection and injection. In order to ensure analytical standards and ensure repeatability, a gas-tight syringe was employed to apply 5 µL of solution directly to the coiled wire. This was left to dry for 3-5 minutes.

Residual products from glassware were diluted in a suitable solvent (methanol or acetonitrile) for on-site screening of laboratory synthesized materials. Once these had been fully dissolved, the tip of the coiled wire was extended and submerged in the solution for 10 seconds (Figure 2).

The coiled wire was then removed from the solution and left to dry for 3-5 minutes in order to minimize any excess solvent entering the system. This was then injected directly into GC/MS for analysis.

Representation of the sample collection and injection process using CME.

Figure 2. Representation of the sample collection and injection process using CME. Image Crdit: PerkinElmer

Table 1. GC/MS Method Parameters. Source: PerkinElmer

. .
Sampling Coiled Microextraction (CME)
Injection Type Splitless
GC Injector Temp. 270 °C
GC Column MXT-5, 5 m x 0.1 mm, 0.4 μm df
GC Column Temp. 50-300°C at 2°C/s, hold for 60 s
GC Carrier Gas Helium, 0.2 mL/min.
Transfer Line Temp. 250°C
Ionization Source In-trap Electron Impact (EI)
Mass Analyzer Toroidal Ion Trap
Mass Range 41 - 500 Da
Detector Electron Multiplier
Resolution <0.5 m/z at 300 amu, nominal unit mass at 500 amu

 

Results and discussion

Figure 3 displays the GC/MS analysis of carfentanil in methanol. The Torion® T-9 was able to successfully detect and positively identify every compound.

An onboard deconvolution algorithm was used to identify fentanyl analogs. This allowed the samples to be positively identified, matching the MS data to the Wiley Designer Drug Library.

CME-GC/MS analysis of 100 mg/mL solution of carfentanil in methanol. (A) TIC of carfentanil. (B) Positive ion mass spectrum of carfentanil, showing the pseudomolecular ion at m/z 395.

Figure 3. CME-GC/MS analysis of 100 mg/mL solution of carfentanil in methanol. (A) TIC of carfentanil. (B) Positive ion mass spectrum of carfentanil, showing the pseudomolecular ion at m/z 395. Image Crdit: PerkinElmer

The Torion T-9® CME-GC/MS method was able to successfully collect, analyze and identify the compounds of interest in forensics scenarios involving synthesized fentanyl analogs and adulterated heroin.

Figure 4 displays CME-GC/MS analysis of a heroin solution containing 5% fentanyl diluted in methanol. This demonstrates the Torion T-9’s ability to screen adulterated solutions.

Figure 5A displays CME-GC/MS analysis of residual products acquired from glassware employed in the synthesis of the fentanyl analogs prepared at the University of North Texas. Here, post-processing and MS matching facilitated the identification of fentanyl that had been collected directly from laboratory glassware.

Figure 5B displays MS data that has been compared to a NIST reference, highlighting the differences between the toroidal ion trap and quadrupole mass analyzers.

Differences in peak intensities coupled with the presence of the pseudo-molecular ion [Fentanyl+H]+ at m/z 337 are a result of the collision-induced dissociations that occur in ion trap mass analyzers.

CME-GC/MS analysis of a heroin solution containing 5% fentanyl in acetonitrile.

Figure 4. CME-GC/MS analysis of a heroin solution containing 5% fentanyl in acetonitrile. Image Crdit: PerkinElmer

CME-GC/MS analysis of glassware used to synthesize fentanyl diluted in acetonitrile. (A) TIC of fentanyl and additional products from the fentanyl synthesis. (B) MS comparison between fentanyl collected with Torion T-9 (Blue) and NIST reference spectra (Red).

Figure 5. CME-GC/MS analysis of glassware used to synthesize fentanyl diluted in acetonitrile. (A) TIC of fentanyl and additional products from the fentanyl synthesis. (B) MS comparison between fentanyl collected with Torion T-9 (Blue) and NIST reference spectra (Red). Image Crdit: PerkinElmer

Conclusions

In the examples presented here, Custodion® Coiled Microextraction (CME) syringes and the Torion T-9® Portable GC/MS were used to collect and identify fentanyl, acetyl fentanyl, carfentanil and heroin in relevant drug screening scenarios.

The CME-GC/MS technique was used in conjunction with the Wiley Designer Drug Library to provide rapid identification of drugs of abuse and new psychoactive substances (NPS).

This process took less than 8 minutes, thanks to its simplified approach and minimal user interaction. Not only does this approach enable effective in-field screening, it also protects users from potentially harmful evidence.

References

  1. World Health Organization. Executive Summary The Selection and Use of Essential Medicines 2017; Geneva, 2017.
  2. United Nations Office on Drugs and Crime. World Drug Report 2017: Global Overview of Drug Demand and Supply. In World Drug Report 2017; 2017; p 68.
  3. Marinetti, L. J.; Ehlers, B. J. A Series of Forensic Toxicology and Drug Seizure Cases Involving Illicit Fentanyl Alone and in Combination with Heroin, Cocaine or Heroin and Cocaine. J. Anal. Toxicol. 2014, 38 (8), 592–598.
  4. Quick, D.; Choo, K.-K. R. Impacts of Increasing Volume of Digital Forensic Data: A Survey and Future Research Challenges. Digit. Investig. 2014, 11 (4), 273–294.
  5. Science, N. A. of. Strengthening Forensic Science in the United States: A Path Forward; National Academies Press: Washington D.C., 2009.

Acknowledgments

Produced from materials originally authored by Ethan McBride and Guido Verbeck from the University of North Texas, and Zachary Lawton from PerkinElmer Inc.

About PerkinElmer

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Last updated: Jun 8, 2021 at 5:05 AM

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