Spectra interference between diquat and paraquat by second derivative spectrophotometry

A rapid and accurate method, combining solid-phase extraction and second-order derivative spectrophotomety approaches, is developed for the simultaneous determination of diquat (DQ) and paraquat (PQ) in blood, tissue and urine samples. Supernatant resulting from the precipitation of protein (with trichloroacetic acid) in plasma and tissue or Amberlite IRA-401 resin treated urine are passed through a mini-column packed with Wakogel gel (Silica gel). Analytes are then eluted with a non-organic solvent, 0.2mol/l HCl solution containing 2mol/l NH(4)Cl. UV spectrum of the eluent in 220-350nm range provides effective screen to detect the presence of DQ and/or PQ. In the presence of DQ or PQ alone, the analyte present is quantitated by conventional zero- or second-order derivative spectrophotometry. The calibration curve in the 0.1-5.0mg/l range for either analyte obeys Beer's law. When both DQ and PQ are present, their concentrations are determined by the peak amplitudes of their respective second-derivative spectra after the addition of alkaline dithionite reagent. Interference is negligible when the DQ/PQ concentration ratio is within the 5.0-0.2 range.Using a 2-ml of sample size, the detection limits for DQ and PQ in plasma are 0.02 and 0.005mg/l. The corresponding detection limits for urine samples (10ml sample size) are 0.004 and 0.001mg/l. Recoveries of DQ and PQ in triplicate plasma and urine samples spiked with 0.5mg/l of analytes are 93 and 85%. The precision of the proposed method resulting from triplicate study of spiked urine samples varies from 3.2 to 4.6% at 0.5mg/l of DQ and PQ, respectively.     

Delimitation of the time of death by immunohistochemical detection of calcitonin.

To improve the possibilities of delimitating the time of death after longer laytime it was examined if this is possible by immunohistochemical detection of calcitonin. The results show that in our examination material the c-cells of the thyroid glands of up to 4-day-old corpses produce a positive immunoreaction towards calcitonin in all cases whereas none of the corpses older than 13 days show such a reaction. This means that in the case of a negative immunoreaction the time of death can be assumed to lie >4 days before the autopsy. The fact that a negative immunoreaction occurred consistently after 13 days leads to the conclusion that when calcitonin has been stained in a specimen, the death of the respective person must lie a maximum of 12 days earlier, whereby these time-limits may change in considerably different surrounding conditions.     

Characterization and differentiation of cyclopropylfentanyl from E-crotonylfentanyl, Z-crotonylfentanyl,and 3-butenylfentanyl

Recently, a sample containing cyclopropylfentanyl was analyzed at this laboratory. Cyclopropylfentanyl began to appear in the United States' illicit drug markets in 2017. Unfortunately, cyclopropylfentanyl presents an analytical challenge due to its mass spectrum being almost identical to that of crotonylfentanyl. There are two possible isomers of crotonylfentanyl, Z- and E- crotonylfentanyl. In order to provide sufficient analytical data to distinguish the two isomers of crotonylfentanyl and cyclopropylfentanyl, crotonylfentanyl was synthesized and fully characterized. Each isomer was analyzed via nuclear magnetic resonance spectroscopy, gas chromatography–mass spectrometry, and Fourier transform infrared spectroscopy. During the synthesis of crotonylfentanyl, an unknown compound was formed. The identification of this compound and the analytical characterization of the two isomers of crotonylfentanyl are presented. Through the comparison of these compounds, it was confirmed that cyclopropylfentanyl can be differentiated from crotonylfentanyl.     

The security of access to accounts under the PSD2

The revised Payment Services Directive (‘PSD2’) has been adopted to stimulate the development of an integrated internal market for payment services. In particular, it facilitates payment initiation services and account information services by granting the providers of these services access to the accounts of the payment service users. At the same time, the recitals state that the PSD2 guarantees a high level of consumer protection, security of payment transactions and protection against fraud.This paper answers the following question: To what extent does the access to accounts of the payment initiation service providers and account information service providers balance the development of the market for payment services with the security of the payment account and the privacy of the user? An analysis of the PSD2 shows that the development of the market for payment services has a higher priority. Security and privacy are ultimately subordinate.First, the PSD2 does not adequately protect the personal data of the users. The definition of ‘account information service’ is broad and covers a wide range of services. This allows the payment service providers to circumvent the limitations of the access to accounts.Next, the payment service providers have a ‘fall back option’ that allows ‘screen scraping’ if the dedicated interface is not functioning properly. Although this access is constrained by several safeguards, the fall back option gives the payment services provider unlimited access to the account of the user.Finally, the payment service providers have considerable freedom to arrange their authentication process as they see fit. The banks seem to be required to trust this process. The PSD2 and regulatory technical standards do not demand that a bank is able to verify the authentication or the integrity of the payment order.     

The importance of dark adaptation for forensic examinations; an evaluation of the Crime-lite Eye™

Forensic practitioners are recommended to dark adapt their eyes prior to conducting evidential searches in the dark. The dark adaptation process remains poorly standardised across the discipline, with little quantified regarding the benefits of such preparative steps. Herein, we report the findings of a study that recruited 50 participants to assess the effectiveness of the Crime-lite Eye?, a darkness adaptation device developed to assist forensic practitioners both in the laboratory and in field. Participants were tasked with searching for the fluorescent signatures left by reaction of 1,8-diazafluoren-9-one (DFO) with amino acids, in a manner akin to the fluorogenic fingerprint treatment of porous evidence. Using an Epson Stylus Photo R265 inkjet printer, ink cartridges were filled with alanine solutions of various concentrations, allowing different motifs to be printed onto copy paper and subsequently developed using DFO. Participants searched for this ‘evidence’ both with and without dark adapted vision. On average, participants were able to locate and correctly recognise 16% more evidence once dark adapted using the Crime-lite Eye?.The increase in evidence located by participants once dark adapted suggests that crime scene officers should be dark adapting in order to visualise as much as possible. The time taken to dark adapt, 10?min on average during this study, is not excessively long, and should not significantly slow the investigation.