Finding evidence at a crime scene: Sensitive determination of benzodiazepine residues in drink and food paraphernalia by HPLC-HRMS/MS

Vincenti, Flaminia; Montesano, Camilla; Babino, Pamela; Carboni, Simona; Napoletano, Sabino; Sangro, Giovanni De; Rosa, Fabiana Di; Gregori, Adolfo; Curini, Roberta; Sergi, Manuel

doi:10.1016/j.forc.2021.100327

Cited by 11 publications

(8 citation statements)

References 16 publications

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“…With regard to liquid chromatographic separation, it was decided to work with a mixed sorbent column on the basis of previous experiences with this family of compounds [ 20 ]. The mobile phases were selected thanks to the expertise gained in the field of NPS analysis and opioids; in particular, phase A, constituted by 10 mM ammonium formate acidified with 0.1% of HCOOH, was evaluated to perform a better ionization of all target analytes in the H-ESI source, as previously described by Montesano et al [ 20 ], while phase B was chosen since in the literature it is widely demonstrated that mixing different percentages of MeOH and MeCN can improve the chromatographic separation of several types of analytes if compared with the separation provided by the use of single solvents [ 21 ]. Different ratios of the two solvents were tested and the necessary peak resolution was obtained by using MeCN–MeOH with a ratio 50:50 ( v / v ).…”

Section: Resultsmentioning

confidence: 99%

Simultaneous Quantification of 25 Fentanyl Derivatives and Metabolites in Oral Fluid by Means of Microextraction on Packed Sorbent and LC–HRMS/MS Analysis

et al. 2021

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Fentanyl and fentalogs’ intake as drugs of abuse is experiencing a great increase in recent years. For this reason, there are more and more cases in which it is important to recognize and quantify these molecules and related metabolites in biological matrices. Oral fluid (OF) is often used to find out if a subject has recently used a psychoactive substance and if, therefore, the person is still under the effect of psychotropics. Given its difficulty in handling, good sample preparation and the development of instrumental methods for analysis are essential. In this work, an analytical method is proposed for the simultaneous determination of 25 analytes, including fentanyl, several derivatives and metabolites. OF was collected by means of passive drool; sample pretreatment was developed in order to be fast, simple and possibly semi-automated by exploiting microextraction on packed sorbent (MEPS). The analysis was performed by means of LC–HRMS/MS obtaining good identification and quantification of all the analytes in less than 10 min. The proposed method was fully validated according to the Scientific Working Group for Forensic Toxicology (SWGTOX) international guidelines. Good results were obtained in terms of recoveries, matrix effect and sensitivity, showing that this method could represent a useful tool in forensic toxicology. The presented method was successfully applied to the analysis of proficiency test samples.

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Section: Resultsmentioning

confidence: 99%

Simultaneous Quantification of 25 Fentanyl Derivatives and Metabolites in Oral Fluid by Means of Microextraction on Packed Sorbent and LC–HRMS/MS Analysis

et al. 2021

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“…Nonetheless, semi-quantitative determination of benzodiazepines from different surfaces of items found in crime scenes of DFCs has also been reported [32].…”

Section: Introductionmentioning

confidence: 99%

“…Dispersive liquid-liquid microextraction (DLLME) has been proposed as a sample pretreatment procedure in many fields owing to its fast, simple, limited use of a large volume of solvent, and its high extraction efficiency [33]. DLLME has been used for the extraction of methamphetamine, opioids, hallucinogens, cannabinoids [34], benzodiazepines [32,35], and GHB [36]. In this study, we established the quantitative determination of ketamine, nimetazepam, and xylazine through simulating the three possible forms of samples in suspected spiked beverages.…”

Section: Introductionmentioning

confidence: 99%

“…Admittedly, several studies have attempted to detect residues of gamma hydroxybutyrate (GHB) [30], ketamine [4, 27], flunitrazepam [7], and diazepam [31]; however, these studies were limited to qualitative determination. Nonetheless, semi‐quantitative determination of benzodiazepines from different surfaces of items found in crime scenes of DFCs has also been reported [32].…”

Section: Introductionmentioning

confidence: 99%

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Vortex‐assisted dispersive liquid–liquid microextraction‐gas chromatography (VADLLME‐GC) determination of residual ketamine, nimetazepam, and xylazine from drug‐spiked beverages appearing in liquid, droplet, and dry forms

Teoh

Sadiq

Saisahas

et al. 2022

Journal of Forensic Sciences

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Presently, investigations of drug‐facilitated crimes (DFCs) rely on the detection of substances extracted from biological samples following intake by the victim. However, such detection requires rapid sampling and analysis prior to metabolism and elimination of the drugs from the body. In cases of suspected DFCs, drug‐spiked beverage samples, whether in liquid, droplet, or even dried form, can be tested for the presence of spike drugs and used as evidence for the occurrence of DFCs. This study aimed to quantitatively determine three sedative‐hypnotics (ketamine, nimetazepam, and xylazine) from drug‐spiked beverages using a vortex‐assisted dispersive liquid–liquid microextraction‐gas chromatography (VADLLME‐GC) approach. In this study, a GC method was first developed and validated, followed by the optimization of the VADLLME protocol, which was then applied to quantify the target substances in simulated forensic case scenarios. The developed GC method was selective, sensitive (limit of detection: 0.08 μg/ml [ketamine]; 0.16 μg/ml [nimetazepam]; 0.08 μg/ml [xylazine]), linear (R2 > 0.99), precise (%RSD <7.2%), and accurate (% recovery: 92.8%–103.5%). Higher recoveries were achieved for the three drugs from beverage samples in liquid form (51%–97%) as compared to droplet (48%–96%) and dried (44%–93%) residues. The recovery was not hindered by very low volumes of spiked beverage and dried residues. In conclusion, the developed VADLLME‐GC method successfully recovered ketamine, nimetazepam, and xylazine from spiked beverages that are likely to be encountered during forensic investigation of DFCs.

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“…Such evidence would appear in dry form due to complete consumption of beverages by victims or delay in forensic analysis. Several studies have successfully proven the possibility of detecting spiked drugs although the beverage residue appeared in dried form [4,5,[24][25][26][27][28].…”

Section: Introductionmentioning

confidence: 99%

Detection and discrimination of sedative‐hypnotics in spiked beverage dry residues using attenuated total reflectance‐Fourier transform infrared (ATR‐FTIR) spectroscopy combined with chemometrics

Teoh

Sadiq

Saisahas

et al. 2022

Journal of Forensic Sciences

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Drugs-facilitated crimes (DFCs) involve the incapacitation of victims under the influence of drugs. Conventionally, a drug administration act is often determined through the examination of biological samples; however, dry residues from any surface, such as drinking glass if related to a DFC could be a potential source of evidence. This study was aimed to establish an attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy coupled with chemometrics for the determination of spiked sedative-hypnotics from dry residues of a drug-spiked beverage. In this study, four sedative-hypnotics, namely diazepam, ketamine, nimetazepam, and xylazine were examined using ATR-FTIR spectroscopy. Subsequently, the ATR-FTIR profiles were compared and decomposed by principal component analysis (PCA) followed by linear discriminant analysis (LDA) for their detection and discrimination. Visual comparison of ATR-FTIR profiles revealed distinct spectra among the tested drugs. An initial unsupervised exploratory PCA model indicated the separation of four main sedativehypnotics clusters, and the proposed PCA score-LDA model had allowed for a 100% accurate classification. Discrimination of sedative-hypnotics from a dry beverage previously spiked with these drugs was also possible upon an additional extraction procedure. In conclusion, ATR-FTIR coupled with PCA score-LDA model was useful in detecting and discriminating sedative-hypnotics, including those that had been previously spiked into a beverage.

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Finding evidence at a crime scene: Sensitive determination of benzodiazepine residues in drink and food paraphernalia by HPLC-HRMS/MS

Cited by 11 publications

References 16 publications

Simultaneous Quantification of 25 Fentanyl Derivatives and Metabolites in Oral Fluid by Means of Microextraction on Packed Sorbent and LC–HRMS/MS Analysis

Simultaneous Quantification of 25 Fentanyl Derivatives and Metabolites in Oral Fluid by Means of Microextraction on Packed Sorbent and LC–HRMS/MS Analysis

Vortex‐assisted dispersive liquid–liquid microextraction‐gas chromatography (VADLLME‐GC) determination of residual ketamine, nimetazepam, and xylazine from drug‐spiked beverages appearing in liquid, droplet, and dry forms

Detection and discrimination of sedative‐hypnotics in spiked beverage dry residues using attenuated total reflectance‐Fourier transform infrared (ATR‐FTIR) spectroscopy combined with chemometrics

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