scholarly journals Structural modification of fentanyls for their retrospective identification by gas chromatographic analysis using chloroformate chemistry

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Carlos A. Valdez ◽  
Roald N. Leif ◽  
Robert D. Sanner ◽  
Todd H. Corzett ◽  
Mark L. Dreyer ◽  
...  

AbstractThe one-step breakdown and derivatization of a panel of nine fentanyls to yield uniquely tagged products that can be detected by Electron Ionization Gas Chromatography-Mass Spectrometry (EI-GC-MS) is presented. The method involves the treatment of the synthetic opioids with 2,2,2-trichloroethoxycarbonyl chloride (TrocCl) at 60 °C for 3 h in dichloromethane and furnishes two products from one fentanyl molecule that can be used to retrospectively identify the original opioid. Parameters that were studied and fully optimized for the method included temperature, solvent, nature of scavenging base and reaction time. One of the two resulting products from the reaction bears the trichloroethoxycarbonyl (Troc) tag attached to the norfentanyl portion of the original opioid and greatly aids in the opioid detection and identification process. The methodology has been applied to the chemical modification of a panel of nine fentanyls and in all cases the molecular ion peak for the Troc-norfentanyl product bearing the distinctive trichloroethyl isotopic signature can be clearly observed. The method’s LLOD was determined to be 10 ng/mL while its LLOQ was found to be 20 ng/mL. This methodology represents the first application of chloroformates in the chemical modification of this class of synthetic opioids that are notoriously inert to common derivatization strategies available for GC–MS analysis.

2020 ◽  
Vol 27 (10) ◽  
pp. 1616-1633 ◽  
Author(s):  
Oana Cristina Duta ◽  
Aurel Mihail Ţîţu ◽  
Alexandru Marin ◽  
Anton Ficai ◽  
Denisa Ficai ◽  
...  

Polymeric materials, due to their excellent physicochemical properties and versatility found applicability in multiples areas, including biomaterials used in tissue regeneration, prosthetics (hip, artificial valves), medical devices, controlled drug delivery systems, etc. Medical devices and their applications are very important in modern medicine and the need to develop new materials with improved properties or to improve the existent materials is increasing every day. Numerous reasearches are activated in this domain in order to obtain materials/surfaces that does not have drawbacks such as structural failure, calcifications, infections or thrombosis. One of the most used material is poly(vinylchloride) (PVC) due to its unique properties, availability and low cost. The most common method used for obtaining tubular devices that meet the requirements of medical use is the surface modification of polymers without changing their physical and mechanical properties, in bulk. PVC is a hydrophobic polymer and therefore many research studies were conducted in order to increase the hydrophilicity of the surface by chemical modification in order to improve biocompatibility, to enhance wettability, reduce friction or to make lubricious or antimicrobial coatings. Surface modification of PVC can be achieved by several strategies, in only one step or, in some cases, in two or more steps by applying several techniques consecutively to obtain the desired modification / performances. The most common processes used for modifying the surface of PVC devices are: plasma treatment, corona discharge, chemical grafting, electric discharge, vapour deposition of metals, flame treatment, direct chemical modification (oxidation, hydrolysis, etc.) or even some physical modification of the roughness of the surface.


2020 ◽  
Vol 24 (4) ◽  
pp. 465-471 ◽  
Author(s):  
Zita Rádai ◽  
Réka Szabó ◽  
Áron Szigetvári ◽  
Nóra Zsuzsa Kiss ◽  
Zoltán Mucsi ◽  
...  

The phospha-Brook rearrangement of dialkyl 1-aryl-1-hydroxymethylphosphonates (HPs) to the corresponding benzyl phosphates (BPs) has been elaborated under solid-liquid phase transfer catalytic conditions. The best procedure involved the use of triethylbenzylammonium chloride as the catalyst and Cs2CO3 as the base in acetonitrile as the solvent at room temperature. The substrate dependence of the rearrangement has been studied, and the mechanism of the transformation under discussion was explored by quantum chemical calculations. The key intermediate is an oxaphosphirane. The one-pot version starting with the Pudovik reaction has also been developed. The conditions of this tandem transformation were the same, as those for the one-step HP→BP conversion.


2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Babacar Faye ◽  
Mouhamed Sarr ◽  
Khaly Bane ◽  
Adjaratou Wakha Aidara ◽  
Seydina Ousmane Niang ◽  
...  

This study evaluated the one-year clinical performance of a one-step, self-etch adhesive (Optibond All-in-One, Kerr, CA, USA) combined with a composite (Herculite XRV Ultra, Kerr Hawe, CA, USA) to restore NCCLs with or without prior acid etching. Restorations performed by the same practitioner were evaluated at baseline and after 3, 6, and 12 months using modified USPHS criteria. At 6 months, the recall rate was 100%. The retention rate was 84.2% for restorations with prior acid etching, but statistically significant differences were observed between baseline and 6 months. Without acid etching, the retention rate was 77%, and no statistically significant difference was noted between 3 and 6 months. Marginal integrity (93.7% with and 87.7% without acid etching) and discoloration (95.3% with and 92.9% without acid etching) were scored as Alpha or Bravo, with better results after acid etching. After one year, the recall rate was 58.06%. Loss of pulp vitality, postoperative sensitivity, or secondary caries were not observed. After one year retention rate was of 90.6% and 76.9% with and without acid conditioning. Optibond All-in-One performs at a satisfactory clinical performance level for restoration of NCCLs after 12 months especially after acid etching.


2021 ◽  
Author(s):  
Dennis Larsen ◽  
Sophie R. Beeren

Template-induced kinetic trapping of specific cyclodextrins in enzyme-mediated dynamic combinatorial libraries of linear and cyclic α-glucans enables the one-step synthesis of cyclodextrins from maltose in water.


Plants ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 77
Author(s):  
Elena O. Vidyagina ◽  
Nikolay N. Kharchenko ◽  
Konstantin A. Shestibratov

Axillary buds of in vitro microshoots were successfully frozen at –196 °C by the one-step freezing method using the protective vitrification solution 2 (PVS2). Microshoots were taken from 11 transgenic lines and three wild type lines. Influence of different explant pretreatments were analyzed from the point of their influence towards recovery after cryopreservation. It was found out that the use of axillary buds as explants after removal of the apical one increases recovery on average by 8%. The cultivation on growth medium of higher density insignificantly raises the regenerants survival rate. Pretreatment of the osmotic fluid (OF) shows the greatest influence on the survival rate. It leads to the increase in survival rate by 20%. The cryopreservation technology providing regenerants average survival rate of 83% was developed. It was based on the experimental results obtained with explant pretreatment. Incubation time in liquid nitrogen did not affect the explants survival rate after thawing. After six months cryostorage of samples their genetic variability was analyzed. Six variable simple sequence repeat (SSR) loci were used to analyze genotype variability after the freezing-thawing procedure. The microsatellite analysis showed the genetic status identity of plants after cryopreservation and of the original genotypes. The presence of the recombinant gene in the transgenic lines after cryostorage were confirmed so as the interclonal variation in the growth rate under greenhouse conditions. The developed technique is recommended for long-term storage of various breeding and genetically modified lines of aspen plants, as it provides a high percentage of explants survival with no changes in genotype.


2021 ◽  
Vol 20 (5) ◽  
Author(s):  
Paweł J. Szabłowski

AbstractWe analyze the mathematical structure of the classical Grover’s algorithm and put it within the framework of linear algebra over the complex numbers. We also generalize it in the sense, that we are seeking not the one ‘chosen’ element (sometimes called a ‘solution’) of the dataset, but a set of m such ‘chosen’ elements (out of $$n>m)$$ n > m ) . Besides, we do not assume that the so-called initial superposition is uniform. We assume also that we have at our disposal an oracle that ‘marks,’ by a suitable phase change $$\varphi $$ φ , all these ‘chosen’ elements. In the first part of the paper, we construct a unique unitary operator that selects all ‘chosen’ elements in one step. The constructed operator is uniquely defined by the numbers $$\varphi $$ φ and $$\alpha $$ α which is a certain function of the coefficients of the initial superposition. Moreover, it is in the form of a composition of two so-called reflections. The result is purely theoretical since the phase change required to reach this heavily depends on $$\alpha $$ α . In the second part, we construct unitary operators having a form of composition of two or more reflections (generalizing the constructed operator) given the set of orthogonal versors. We find properties of these operations, in particular, their compositions. Further, by considering a fixed, ‘convenient’ phase change $$\varphi ,$$ φ , and by sequentially applying the so-constructed operator, we find the number of steps to find these ‘chosen’ elements with great probability. We apply this knowledge to study the generalizations of Grover’s algorithm ($$m=1,\phi =\pi $$ m = 1 , ϕ = π ), which are of the form, the found previously, unitary operators.


2021 ◽  
pp. 153062
Author(s):  
Yue Zhang ◽  
Xinpeng Liu ◽  
Yanan Wang ◽  
Yinan Zhang ◽  
Junwei Wang ◽  
...  
Keyword(s):  
One Step ◽  

Sign in / Sign up

Export Citation Format

Share Document