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Ecstasy (MDMA) Vrsar

MDMA (Ecstasy) Addiction: Signs Of Abuse And Treatment Options

Ecstasy (MDMA) Vrsar

Mephedrone Negombo

Кокаин Греция

Ecstasy (MDMA) Vrsar

Закладки шишки, бошки, гашиш Варадеро

In recent years, ecstasy trafficking has grown in complexity and tablets has been commonly sold containing different contents of 3,4-methylenedioxymethamphetamine MDMA or even other psychoactive substances. In contrast, identification and quantification of drugs of abuse is still a challenge, once the access to drug standards is very restricted in Brazil. In this work, ecstasy tablets seized by the Brazilian Federal Police have their chemical composition identified and quantified by gas chromatography and quantitative 1 H nuclear magnetic resonance based on an internal standard approach IS- 1 H-qNMR. Both methods were validated and showed suitable results for the figures of merit. Comparatively, IS- 1 H-qNMR is more efficient and versatile than gas chromatography to accomplish in a single analysis the identification and quantification of target analytes. Since the method does not require a specific reference material, it is cost effective and provides agility to routine forensic analysis. HCl , which vary in shapes, dimensions, colors, and logos. In recent years, the ecstasy trafficking has grown in complexity and diversification. The addition of other amphetamine type substances ATS became a common practice and substances such as 3,4-methylenedioxyethylamphetamine MDEA , 3,4-methylenedioxyamphetamine MDA , and other chemicals classes, such as piperazines or cathinones, are occasionally detected. A study on the composition of ecstasy tablets in Brazil, carried out on samples from different seizures from August to July showed a strong tendency in tablet adulteration. Forensic Sci. Despite seizures of ATS are generally less frequent in Latin America than in other global markets, considerable amounts were seized in Brazil in kg and kg. This scenario is associated with the unregulated and illegal activity, 3 3 Bell, S. The chemical profiling analysis allows, for example, the comparison of samples similarity, indication of geographic origin, definition of distribution networks, evaluation of synthetic routes, and other valuable information to law enforcement agencies. On the other hand, the determination of ecstasy purity can also be conducted by methods that do not involve a separation step, such as near infrared spectroscopy NIR and quantitative nuclear magnetic resonance of hydrogen 1 H-qNMR. Justice , 46, Actually, the 1 H-qNMR spectroscopy could be more explored as an important tool in forensic science, since it provides a direct proportionality between a signal area and the number of nuclei responsible for that signal. As a result, the technique does not require a reference standard containing the target analyte, which is, in the case of illicit drugs in developing countries, not always readily available, extremely expensive and difficult to obtain. Besides that, NMR can simultaneously perform the identification and quantification of other substances also present in ecstasy tablets, like adulterants, that is still a challenge in forensic drug analysis. Finally, the validated method was applied to a set of ecstasy tablets seized by Brazilian Federal Police. All chemicals were of analytical grade or better and used without additional purification procedures. Dipentylphthalate Maleic acid MA, The MDMA. HCl certified standard Before analysis, tablets were manually crushed in mortar into fine powders. Quantitative analyses were a routine practice in the Brazilian Federal Police laboratory to study the cocaine profile 12 12 Maldaner, A. Freshly prepared solutions were transferred to 2 mL glass vials and sealed for further gas chromatography injection. Homogenized seized samples were used to evaluate some of the figures of merit in validation stages e. HCl standards. Helium was used as the carrier gas at constant flow rate of 1. The total analysis time was 12 min. The Grubbs test was applied for outliers identification. GC-FID was used to identify other active ingredients, like adulterants, on seized ecstasy tablets. HCl certified reference material was also used to verify some figures of merit. The powders were mixed in 1. About 1 mL of the clear upper solution was carefully transferred with a pipette to the NMR tubes. Lock and shimming adjustments were done automatically for all samples. Tuning and matching adjustment were done manually. To avoid sidebands and minimize eventual signal overlapping all 1 H spectra were acquired without sample spinning and with 13 C decoupling during acquisition zgig30 pulse sequence. To ensure complete relaxation, all acquisitions were made with a relaxation delay of at least 10 times the largest T 1 spin-lattice relaxation time value. For determination of the relaxation delay value, T 1 measures of all analytes were previously performed by inversion-recovery experiments. Fourier transformation FT was applied after zero filling the data to 64 k time domain points. The acquired NMR spectra were manually phase-corrected and baseline was automatically set with fifth order polynomial function. The spectra were referenced by TSP- d 4 sodium-2,2,3,3- d 4 trimethylsilylpropionate signal 0 ppm and integrations were manually made using Bruker Topspin 3. For quantification, a well-known equation was applied, which includes the molar weight, integral area, number of protons of the reference compound and analyte, as well as purity and gravimetric mass of the reference. Grubbs test was applied for outliers identification 13 13 Cesar, I. An analytical curve was plotted for MDMA. HCl concentrations ranging from 0. The method was considered linear over the entire studied concentration range. The method is also precise in terms of repeatability same analyst, same day, six replicates at three levels of MDMA concentration and intermediate precision same analyst and equipment in different days; same equipment in the same day by different analysts; same analyst in the same day and in different equipment. HCl purity with certified standard mixtures with cellulose and robust for all variables evaluated flow rate, injector temperature, oven temperature, split ratio, injection volume. The limits of detection and quantification and the combined standard uncertainty are adequate for the proposed application. The potential interference of some traditional ATS MDEA, MDA and amphetamine and pharmaceutical adulterants paracetamol, caffeine, mephedrone, benzocaine, phenacetin, lidocaine, aminopyrine, levamisole and procaine present in ecstasy tablets was also evaluated. Currently, this method is part of the quality assurance system of Brazilian Federal Police laboratory and has been used routinely. Initially, MA and DMS solutions were used as reference to evaluate the figures of merit of a general method for quantitative analysis by 1 H-qNMR using internal standard. Once satisfactory results were achieved, the particularities for quantification of MDMA. For this purpose, the integral values of MA 6. The residues obtained are small less than 0. The IS- 1 H-qNMR method shows good precision results in all three tests equipment repeatability, method repeatability and intermediate precision. Therefore, they do not affect the results of quantification by IS- 1 H-qNMR and the method is considered robust in regard to acquisition and processing of the parameters investigated. Solutions containing MA and DMS are stable for at least 20 days at room temperature, since subsequent analyses show relative errors below 0. The combined standard uncertainty calculation takes into account contributions from all important uncertainty sources, like gravimetric mass and molecular weight of MA and DMS, purity of MA, integral ratio of MA and DMS and recovery. The combined standard uncertainty was 0. This result is expected once recovery is actually a combination of various factors, such as sample preparation and purity of internal standard and analyte. The uncertainty estimation of the 1 H-qNMR method presents acceptable value and corroborates the power of this technique when combined with careful sample preparation. HCl quantification. Complete assignment of MDMA. The signal of the methylenedioxy group 5. HCl, since it is a singlet in a relatively quiet region, reducing the possibility of interference, and it can be used to discriminate MDMA. HCl from other ATS, such as methamphetamine and amphetamine. HCl 5. This is shown in Figure S2 SI section. In addition, MDMA. The precision of the method was also determined for MDMA. HCl 3 replicates and showed an RSD value of 1. The accuracy experiments previously performed with DMS cannot be directly applied for solutions of different analytes or solvents. A good recovery depends on the extraction step, which is particularly critical in samples with lower purity, and recovery experiments must be designed considering matrix complexity. HCl analyte. HCl concentration determined in real samples. The stability of MDMA. HCl and MA solutions in D 2 O was also assessed using the solutions prepared for recovery experiment. Solutions were analyzed, stored at room temperature in NMR tubes and analyzed again in 72 h. HCl determination. The contribution of each component gravimetric mass, molecular weight, purity of internal standard, integral ratio of analyte and internal standard and recovery was calculated considering the square of the standard uncertainty. The result shows that recovery is again the main factor for NMR uncertainty Seizures were separated in 38 batches according to geographical origin, apprehension date and physical characteristics e. The seized tablets present seventeen different logos, weights between and mg and five different excipients were identified by FTIR analysis cellulose, sucrose, starch, talc, and fatty esters of long chain. The curve presents an adequate correlation with slope of 0. Moreover, the residues values are randomized and show neither bias nor curvatures. Therefore, the results obtained by the two methods can be considered statistically equal. The sample preparation is simple, fast and convenient. Since it is not necessary to prepare specific analytical curves, this method demands less work and time. Besides that, the possibility of NMR to identify virtually any active substance of an illegal drug and to quantify it without using the standard of the target analyte are the major advantages of this technique when compared to the commonly used chromatographic methods. In fact, once the method does not demand for specific certified reference material, it can be applied to reduce costs and to provide agility for forensic analysis, which always handles urgency in results and faces unpredictable samples composition. The authors would like to thank the Brazilian Federal Police, the U. Abrir menu Brasil. Journal of the Brazilian Chemical Society. Abrir menu. Nathalia S. Experimental Chemical and reagents All chemicals were of analytical grade or better and used without additional purification procedures. The letters identify hydrogens of MDMA molecular structure. Togni, L. Bell, S. Cole, J. Gimeno, P. Van Deursen, M. Justice , 46 , Maldaner, A. Publication Dates Publication in this collection Sept History Received 15 Dec Accepted 3 Apr This is an Open Access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Luiz E. Adriano O. Aline L. Figures 3 Tables 1. RSD: relative standard deviation. Google Google Scholar.

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Ecstasy (MDMA) Vrsar

Экстази (МДМА) Тбилиси