scholarly journals Optimized and Validated DBS/MAE/LC–MS Method for Rapid Determination of Date-Rape Drugs and Cocaine in Human Blood Samples—A New Tool in Forensic Analysis

Separations ◽  
2021 ◽  
Vol 8 (12) ◽  
pp. 249
Author(s):  
Paweł Stelmaszczyk ◽  
Ewa Gacek ◽  
Renata Wietecha-Posłuszny
Keyword(s):  
Date Rape ◽  
Rapid Determination ◽  
Extraction Process ◽  
Forensic Analysis ◽  
Blood Samples ◽  
Assisted Extraction ◽  
Wide Range ◽  
Human Blood Samples ◽  
Date Rape Drugs

The aim of this work was to develop a new method for the determination of selected substances from the date-rape drugs group: ketamine, benzodiazepines and cocaine. The method is based on the dried blood spot method which seems to be a suitable tool in the analysis of tested substances. The extraction process based on microwave-assisted extraction was optimized to enable optimal conditions for the isolation of a wide range of analytes from blood samples collected on DBS cards. The extraction with ethyl acetate with a buffer of pH = 9 carried out at a temperature of 50 °C for 15 min ensured high extraction efficiency of the tested analytes. The optimized method was validated. Limits of detection (LOD = 4.38–21.1 ng/mL) and quantification (LOQ = 14.6–70.4 ng/mL), inter- and intra-day precision (CV = 1.37–13.4% and 3.39–14.8%, respectively), recovery (RE = 93.0–112.4%) and matrix effect (ME = 98.4–101.6%) were determined. The validation results indicate the possibility of using the proposed method in the analysis of real blood samples collected from victims of sexual assault.

Rapid Determination of H2S Poisoning in a Forensic Study Using a Novel Fluorescence Assay Based on Zn/Cu@BSA Nanoclusters

2018 ◽  
Vol 71 (3) ◽  
pp. 142 ◽  
Author(s):  
Lagabaiyila Zha ◽  
Weicheng Duan ◽  
Di Wen ◽  
Yadong Guo ◽  
Jie Yan ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Forensic Analysis ◽  
Gas Chromatography Mass Spectrometry ◽  
Metal Nanoclusters ◽  
Fluorescence Sensing ◽  
Blood Samples ◽  
H2s Poisoning

The quantitative determination of H2S in the blood can provide valid evidence for H2S poisoning through occupational exposure. However, known traditional methods for the detection of H2S in blood are time consuming, require complicated pretreatments, and have low sensitivity. In this paper, a new fluorescence sensing assay is proposed for the rapid detection of H2S poisoning in forensic cases based on bovine serum albumin (BSA)-stabilised zinc/copper (Zn/Cu) bi-metal nanoclusters (Zn/Cu@BSA NCs). The as-prepared Zn/Cu@BSA NCs probes have been characterised by UV-vis absorption and fluorescence spectroscopy. The fluorescence of Zn/Cu@BSA NCs can be quenched through specific interactions between HS−/S2− and the Zn2+/Cu2+ bi-metal ions. Under optimised conditions, the fluorescence sensing method was linear in the concentration range of 2.5 nM to 30 mM with 0.69 nM as the limit of detection. Moreover, the practical feasibility of this fluorescence sensing method has also been demonstrated by the analysis of mice blood samples containing different levels of sulfide and human blood samples from forensic cases of H2S poisoning. Compared with gas chromatography/mass spectrometry (GC/MS), this fluorescence sensing method is quite simple, straightforward, and can be accurate for the quantitative determination of H2S poisoning in a few minutes for forensic analysis. Overall, this is the first report of a bi-metal fluorescence sensing assay for detecting H2S poisoning directly in blood. This research may provide a new approach for forensic toxicologists to monitor poisoning by H2S using a fluorescence-sensing method.

scholarly journals The Double Face of Ketamine—The Possibility of Its Identification in Blood and Beverages

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 813
Author(s):  
Magdalena Świądro ◽  
Paweł Stelmaszczyk ◽  
Irena Lenart ◽  
Renata Wietecha-Posłuszny
Keyword(s):  
Date Rape ◽  
Signal To Noise Ratio ◽  
High Sensitivity ◽  
Heroin Addiction ◽  
Assisted Extraction ◽  
Low Concentrations ◽  
High Concentrations ◽  
Rosé Wine ◽  
Tof Ms

The purpose of this study was to develop and validate a high-sensitivity methodology for identifying one of the most used drugs—ketamine. Ketamine is used medicinally to treat depression, alcoholism, and heroin addiction. Moreover, ketamine is the main ingredient used in so-called “date-rape” pills (DRP). This study presents a novel methodology for the simultaneous determination of ketamine based on the Dried Blood Spot (DBS) method, in combination with capillary electrophoresis coupled with a mass spectrometer (CE-TOF-MS). Then, 6-mm circles were punched out from DBS collected on Whatman DMPK-C paper and extracted using microwave-assisted extraction (MAE). The assay was linear in the range of 25–300 ng/mL. Values of limits of detection (LOD = 6.0 ng/mL) and quantification (LOQ = 19.8 ng/mL) were determined based on the signal to noise ratio. Intra-day precision at each determined concentration level was in the range of 6.1–11.1%, and inter-day between 7.9–13.1%. The obtained precision was under 15.0% (for medium and high concentrations) and lower than 20.0% (for low concentrations), which are in accordance with acceptance criteria. Therefore, the DBS/MAE/CE-TOF-MS method was successfully checked for analysis of ketamine in matrices other than blood, i.e., rose wine and orange juice. Moreover, it is possible to identify ketamine in the presence of flunitrazepam, which is the other most popular ingredient used in DRP. Based on this information, the selectivity of the proposed methodology for identifying ketamine in the presence of other components of rape pills was checked.

scholarly journals Rapid Determination of Ethylene Oxide and 75 VOCs in Ambient Air with Canister Sampling and Associated Growth Issues

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 35
Author(s):  
Jason Hoisington ◽  
Jason S. Herrington
Keyword(s):  
Ethylene Oxide ◽  
Rapid Determination ◽  
Complex Mixture ◽  
Ambient Air ◽  
Gas Chromatography Mass Spectrometry ◽  
Average Accuracy ◽  
Relative Standard ◽  
Wide Range ◽  
Us Epa

A canister-based sampling method along with preconcentrator-Gas chromatography-Mass Spectrometry (GC-MS) analysis was applied to ethylene oxide (EtO or EO) and 75 other volatile organic compounds (VOCs) in ambient air. Ambient air can contain a large variety of VOCs, and thorough analysis requires non-discriminatory sampling and a chromatographic method capable of resolving a complex mixture. Canister collection of whole air samples allows for the collection of a wide range of volatile compounds, while the simultaneous analysis of ethylene oxide and other VOCs allows for faster throughput than separate methods. The method presented is based on US EPA Method TO-15A and allows for the detection of EtO from 18 to 2500 pptv. The method has an average accuracy of 104% and precision of 13% relative standard deviation (RSD), with an instrument run time of 32 min. In addition, a link between canister cleanliness and ethylene oxide growth is observed, and potential mechanisms and cleaning strategies are addressed.

Optimized liquid-chromatographic determination of metronidazole and its metabolites in plasma.

1984 ◽  
Vol 30 (5) ◽  
pp. 784-787 ◽  
Author(s):  
R A Gibson ◽  
L Lattanzio ◽  
H McGee
Keyword(s):  
Rapid Determination ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Detector Response ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Wide Range ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Metronidazole and its known metabolites in plasma can be rapidly separated by a "high-pressure" liquid-chromatographic method that can also be adapted for rapid determination of tinidazole. Samples deproteinized with trichloroacetic acid (50 g/L final concentration) undergo isocratic separation on a reversed-phase C18 column eluted with an 8/92 (by vol) mixture of acetonitrile/KH2PO4 (5 mmol/L, pH 3.0). The method is sensitive, reliably detecting as little as 25 micrograms of metronidazole and (or) its metabolites per milliliter of plasma. The detector response varied linearly with concentration for all compounds tested over a wide range (25-500 micrograms/L). Within-day and between-day variation was generally less than 2.5% for all concentrations of all compounds tested. Various other antibiotics tested did not interfere.

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