Potential 2-Aminoindane Fatality Invalidated by Careful Mass Spectrometric Analysis

Author(s):  
Marine Deville ◽  
Nathalie Dubois ◽  
Corinne Charlier

Abstract We describe herewith the case of a patient presenting to the emergency department for worsening ear–nose–throat symptoms. As chemsex was evocated by the family, patient’s serum was submitted to a new psychoactive substances screening. After a simple liquid–liquid extraction, serum was injected on a high-resolution mass spectrometer using quite usual conditions (C18 column, gradient mode with acidic buffer, methanol and acetonitrile). An almost perfect match with 2-aminoindane (2-AI) was observed considering that the precursor ion was present in the sample but absent in the commercial library. Literature concerning 2-AI is sparse, and further investigations were undertaken. After injection of the reference standard, a small retention time shift has been observed (0.3 min) between the standard and the sample. The case was only closed while spiking the sample with the standard, giving rise to two distinct peaks. As a result, 2-AI was then considered as absent from the sample and death was attributed only to infection. Moreover, a rapid liquid chromatography–tandem mass spectrometry method dedicated to 2-AI was developed. It generated the same false-positive result highlighted by significant differences observed in ion ratios (2.37 for the sample versus 6.62 for the neat standard).

Author(s):  
Ana Carolina Furiozo Arantes ◽  
Kelly Francisco da Cunha ◽  
Marilia Santoro Cardoso ◽  
Karina Diniz Oliveira ◽  
Jose Luiz Costa

Abstract Purpose We developed and validated a method for quantitative analysis of 50 psychoactive substances and metabolites (antidepressants, benzodiazepines and opioids) in oral fluid samples using simple liquid–liquid extraction procedure followed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). Method Oral fluid samples were collected using Quantisal™ device and extracted by liquid–liquid extraction with 1.0 mL of methyl tert-butyl ether and then analyzed using LC–MS/MS. Results The method attended method validation criteria, with limits of quantification as low as 0.5 and 1.0 ng/mL, and linearity between 0.5–50.0 ng/mL for antidepressants, 0.5–25.0 ng/mL for benzodiazepines and 1.0–50.0 ng/mL to opioids. During method validation, bias and imprecision values were not greater than 16 and 20%, respectively. Ionization suppression/enhancement bias results were not greater than 25%. No evidence of carryover was observed. Sample stability studies showed that almost all analytes were stable at 25 °C for 3 days and at 4 °C for 7 days. Freeze–thaw cycles stability showed that most antidepressants and opioids were stable under these conditions. Autosampler stability study showed that all analytes were stable for 24 h, except for nitrazepam and 7-aminoclonazepam. Thirty-eight authentic oral fluid samples were analyzed; 36.8% of the samples were positive for 2 drugs. Citalopram was the most common drug found, followed by venlafaxine. Conclusions The method was validated according to international recommendations for the 50 analytes, showing low limits of quantification, good imprecision and bias values, using simple liquid–liquid extraction, and was successfully applied to authentic oral fluid samples analysis.


2019 ◽  
Vol 15 (4) ◽  
pp. 312-318
Author(s):  
Shuoye Yang

Background: The therapeutic ability and application of antifungal peptide (APs) are limited by their physico-chemical and biological properties, the nano-liposomal encapsulation would improve the in vivo circulation and stability. </P><P> Objective: To develop a long-circulating liposomal delivery systems encapsulated APs-CGA-N12 with PEGylated lipids and cholesterol, and investigated through in vivo pharmacokinetics. Methods: The liposomes were prepared and characterized, a rapid and simple liquid chromatographytandem mass spectrometry (LC-MS/MS) assay was developed for the determination of antifungal peptide in vivo, the pharmacokinetic characteristics of APs liposomes were evaluated in rats. Results: Liposomes had a large, unilamellar structure, particle size and Zeta potential ranged from 160 to 185 nm and -0.55 to 1.1 mV, respectively. The results indicated that the plasma concentration of peptides in reference solutions rapidly declined after intravenous administration, whereas the liposomeencapsulated ones showed slower elimination. The AUC(0-∞) was increased by 3.0-fold in liposomes in comparison with standard solution (20 mg·kg-1), the half-life (T1/2) was 1.6- and 1.5-fold higher compared to the reference groups of 20 and 40 mg·kg-1, respectively. Conclusion: Therefore, it could be concluded that liposomal encapsulation effectively improved the bioavailability and pharmacokinetic property of antifungal peptides.


2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Joo Hee Chung ◽  
Kun Cho ◽  
Seongnyeon Kim ◽  
So Hyeon Jeon ◽  
Jeoung Hwa Shin ◽  
...  

An inter-laboratory study was performed to evaluate the performance of a method developed for the quantification of enrofloxacin in chicken meat. Liquid-liquid extraction combined with a clean-up procedure based on solid-phase extraction followed by a liquid chromatography-tandem mass spectrometric method was used by three individual laboratories. All the investigated results of calibration curves and limits of quantification were within the acceptable range for regulatory testing of enrofloxacin. The three laboratories received blind a certified reference material to analyze in triplicate and assess using statistical analysis. From the results, no statistical differences were found between the laboratories in the precision of the method. Additionally, all the results of the z-score, which is an indication of fixed interval bias criteria for accuracy from the laboratories, fell within the allowable limits (±2σ). Based on this proficiency testing by inter-laboratory comparisons, the analytical method including the sample preparation step was proven to be applicable.


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