Trace level detection of select opioids (fentanyl, hydrocodone, oxycodone, and tramadol) in suspect pharmaceutical tablets using surface‐enhanced Raman scattering (SERS) with handheld devices

Abstract

The opioid crisis in the USA has resulted in over 702,000 overdose fatalities between 1999 and 2017 and can be attributed to over‐prescription of opioids and abuse of synthetic opioids in combination with other illicit drugs. A rapid and sensitive SERS method has been developed for trace detection of opioids including fentanyl, hydrocodone, oxycodone, and tramadol in low‐dosage suspect tablets using two different handheld Raman spectrometers equipped with 785 and 1064 nm lasers. The method involves a micro‐extraction procedure using 10% methanol in deionized water, followed by filtration and addition of colloidal silver and aqueous KBr, resulting in a mixture that can be measured directly via a glass vial. The lowest concentration (Cmin) of fentanyl, tramadol, oxycodone, and hydrocodone standards that yielded a positive match was 250 ng/ml, 5, 10, and 10 μg/ml using the 1064 nm laser device and 100 ng/ml, 1 μg/ml, 500 ng/ml, and 750 ng/ml using the 785 nm laser device, respectively. For the analysis of suspect tablets containing these opioids, the Cmin ranges between 5 and 75 µg/ml for 1064 nm laser device and 1 and 50 µg/ml for 785 nm laser device. The overall positive identification rate for all the opioids studied in the suspect counterfeit tablets analyzed ranged from 80% to 100%. The use of SERS for rapid chemical identification at remote sampling sites, such as international mail facilities (IMFs) and express courier hubs (ECHs), provides a rugged, simple, and practical method applicable for point‐of‐entry sampling and analysis.

DARK Classics in Chemical Neuroscience: Bucinnazine

“…Therefore, the development of new methods of analysis is a mandatory task for further studies. The most common methods applied for the detection of opioids in forensic samples are gas chromatography coupled to mass spectrometry (GC–MS), liquid chromatography coupled to mass spectrometry (LC–MS), and liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS), − although thin-layer chromatography (TLC), Raman spectroscopy, and chromatography with detectors other than MS detectors are also applied. , …”

Rapid determination of eight benzodiazepines in suspected counterfeit pharmaceuticals using surface‐enhanced Raman scattering with handheld Raman spectrometers

“…Samples were first prepared for SERS analysis by extracting the benzodiazepines in tablets and capsules using 10% MeOH in water diluent followed by addition of Ag colloids and aggregating agent. This method has been successfully demonstrated by our group to be effective in detecting a wide range of analytes [24][25][26]. If suitable results were not achieved for a given sample using this method, the sample was prepared for SERS analysis by separating the benzodiazepine of interest from tablet or capsule using 10% ammoniated chloroform followed by addition of 1 N HCl and Au colloids.…”

“…Consequently, we have developed several surface-enhanced Raman scattering (SERS) methods using these handheld devices to lower detection limits and increase the number of APIs that can be detected [24][25][26]. These methods have been used along with other analytical devices at a satellite laboratory stationed outside the IMF in Chicago during a three-month pilot program and will soon be used at the same location when the project transitions to a full operational mode [27].…”

Fentanyl detection and quantification using portable Raman spectroscopy in community drug checking

“…[26] Inherent challenges are in achieving sufficient sensitivity for lowconcentration actives and mitigating fluorescence. Recent interest in using the same instrumentation for SERS provides the potential for ultra-trace detection that could be applied in the identification of fentanyl [27][28][29][30] and its analogues, such as carfentanil. [31] In the context of drug checking, developing protocols that can work directly with powdered samples and without any sample preparation is particularly useful.…”