scholarly journals Extraction-chromatographic determination of narcotic drugs and psychotropic substances in objects of complex matrix composition

2021 ◽  
Vol 65 (4) ◽  
pp. 422-430
Author(s):  
O. N. Mikhniuk ◽  
S. M. Leshchev
Keyword(s):  
Aqueous Solutions ◽  
Sharp Decrease ◽  
Chromatographic Determination ◽  
Matrix Composition ◽  
Gas Chromatography Mass Spectrometry ◽  
Maximum Efficiency ◽  
Psychotropic Substances ◽  
Matrix Components ◽  
Narcotic Drugs

A comparison of the capabilities of two methods for extraction-chromatographic determination of narcotic drugs and psychotropic substances in various objects (syrups, ointments, tablets, herbal mixtures, etc.), the screening methanol method commonly used in the practice of customs and forensic examination and the proposed extraction method based on the use of water phase (in particular, water solutions of salts) for preliminary effective separation of analytes from matrix components was made. In extraction systems of hexane–water, hexane–aqueous solutions of inorganic salts (sodium chloride, dipotassium phosphate and potassium carbonate), chloroform–water, the method of gas chromatography – mass spectrometry was used to determine the distribution constants (P) of organic bases – narcotic drugs and psychotropic substances (N-methylephedrine, methamphetamine, amphetamine, methadone, dihydrocodeine, hydrocodone, oxycodone, ketamine, cocaine zolpidem, fentanyl, harmine, harmaline). Based on the obtained extraction characteristics of analytes and matrix components, the optimal extractants and extraction conditions, which ensure the maximum efficiency of separation of analytes and matrix components, as well as the concentration of the analyte were substantiated. The use of extraction using water and aqueous solutions of salts provides both a sharp decrease in the detection limit (from 10–3 to 10–7 mol/dm3) in comparison with the methanol method and stable working of chromatographic equipment due to the removal of thermally unstable matrix components was shown.

scholarly journals Extraction of medicinal compounds of the benzodiazepines class from aqueous solutions and their following gas chromatographic determination

2021 ◽  
Vol 57 (2) ◽  
pp. 177-184
Author(s):  
O. N. Mikhniuk ◽  
S. M. Leshchev
Keyword(s):  
Aqueous Solutions ◽  
Chromatographic Determination ◽  
Selective Extraction ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatographic Technique ◽  
Psychotropic Substances ◽  
Quantitative Extraction ◽  
Relative Standard ◽  
Distribution Constants ◽  
The Republic

In extraction systems hexane–water, hexane–aqueous solutions of inorganic salts (sodium chloride, dipotassium phosphate and potassium carbonate), chloroform–water using the method of gas chromatography–mass spectrometry, the distribution constants of psychotropic substances, limited to movement through the customs border of the Republic of Belarus – alprazolam, lorazepam, temazepam, and as well as clozapine, a medicinal product permitted for movement, were determined. The greatest dynamics of the growth of the distribution constant versus salt concentration was observed in alprazolam. It was found that replacing hexane with chloroform leads to increasing the distribution constants and the quantitative extraction of all substances. However, for the selective extraction of substances from various objects and the simultaneous removal of matrix components, it is necessary to use the systems as hexane–aqueous solutions of salts or hexane–water. Based on the obtained values of the distribution constants of substances, extraction-chromatographic technique for the determination of organic non­electrolytes (benzodiazepines) in various objects is proposed. Metrological characteristics of the techniques are: relative standard deviation does not exceed 2 %, the range of determined concentrations in solutions is 0,05– 1,00 g/dm3.

scholarly journals EXPERT RESEARCH OF MICROQUANTITIES NARCOTIC, PSYCHOTROPIC SUBSTANCES AND PRECURSORS

2018 ◽  
Vol 18 ◽  
pp. 332-351
Author(s):  
N. Sh. Khalilova ◽  
N. V. Korableva ◽  
V. A. Vetrova ◽  
M. U. Abdullayeva ◽  
Z. U. Usmonaliyeva
Keyword(s):  
High Performance ◽  
Gas Chromatography Mass Spectrometry ◽  
Criminal Cases ◽  
Psychotropic Substances ◽  
Low Concentrations ◽  
Mass Spectrometric Detector ◽  
Sensitivity And Selectivity ◽  
Examination Methods ◽  
Active Substances ◽  
Narcotic Drugs

While investigating and prosecuting criminal cases related to illegal drug trade, psychotropic substances and precursors, microobjects found at the scene of crime, as well as on items related to a crime and its participants, assume ever greater evidentiary. In expert practice, narcotic drugs and psychotropic substances often appear as research objects, that are rarely individual compounds. At that greatest difficulties arise while research of substances that are multicomponent systems and mixtures containing a large number of impurity and ballast substances, as well as low concentrations of active substances. So it is difficult to identify the substance that served as the basis for developing a methodology for the investigation of microquantities of narcotic drugs, psychotropic substances and precursors. Despite the fact that chromatographic analysis is the most common method for the analysis of narcotic drugs, psychotropic substances and precursors, currently due to high information content, sensitivity and selectivity in the world practice of forensic chemical and medical examination, methods of gas chromatography-mass spectrometry (GC-MS) and high performance liquid chromatography with mass spectrometric detector (HPLC-MS) become one of the most widely used. The use of the HPLC-MS method is the most optimal while research on narcotic, psychotropic substances and precursors by reducing the time of sample preparation, since there is no need for the stage of reagents evaporation and receipt of derivatives, and also it is appear possible to identify non-volatile substances that cannot be analyzed by GC-MS. As a result of the performed researches a methods for the criminalistic research of microquantities of certain narcotic drugs (heroin, morphine, opium, methamphetamine, cocaine, etc.), psychotropic substances (clonidine, bromazepam, ketazolam, trihexyphenidyl, methaqualone, barbital, etc.), precursors (pseudoephedrine, ephedrine) and a poison such as scopolamine using GC-MS and HPLC-MS.

Capillary Gas Chromatographic Determination of T-2 Toxin, HT-2 Toxin, and Diacetoxyscirpenol in Cereal Grains

1984 ◽  
Vol 67 (6) ◽  
pp. 1105-1107
Author(s):  
Huguette Cohen ◽  
Michel Lapointe
Keyword(s):  
Electron Capture ◽  
Impact Ionization ◽  
Chromatographic Determination ◽  
Fused Silica ◽  
Electron Capture Detector ◽  
Resolving Power ◽  
Cereal Grains ◽  
Gas Chromatography Mass Spectrometry ◽  
Silica Column

Abstract A capillary gas chromatographic (GC) method using an electron capture detector is described for determining T-2 and HT-2 toxins and diacetoxyscirpenol (DAS) in cereal grains at levels as low as 100 ppb for T-2 and DAS and 50 ppb for HT-2. Samples are extracted with methanol-water according to the Scott method, and further purified on a silica gel cartridge and a cyano column. Heptafluorobutyrylimidazole (HFBI) is added to form the esters of the analytes. Ester(s) of T-2, HT-2 and DAS are separated on a 30 m × 0.32 mm DB-5 fused silica column and measured with a "Ni electron capture detector. Samples were confimed by gas chromatography/mass spectrometry using electron impact ionization and single ion monitoring at the molecular mass of 501.11 m/z for T-2, 665.08 m/z for HT-2, and 502.12 m/z for DAS at 10 000 resolving power. The method was applied to wheat, oats, and barley. Average recoveries ranged from a low of 65% for T- 2 in barley to a high of 99% for DAS in oats.

Chromatographic determination of the oligomer content in aqueous solutions in caprolactam regeneration

1993 ◽  
Vol 24 (5) ◽  
pp. 425-427
Author(s):  
R. N. Nikolov ◽  
N. I. Angelova ◽  
D. I. Pishev
Keyword(s):  
Aqueous Solutions ◽  
Chromatographic Determination

scholarly journals Volatile Profile and Physico-Chemical Analysis of Acacia Honey for Geographical Origin and Nutritional Value Determination

Foods ◽  
2019 ◽  
Vol 8 (10) ◽  
pp. 445 ◽  
Author(s):  
Niculina M. Mădaş ◽  
Liviu A. Mărghitaş ◽  
Daniel S. Dezmirean ◽  
Victorita Bonta ◽  
Otilia Bobiş ◽  
...  
Keyword(s):  
Geographical Origin ◽  
Solid Phase ◽  
Chromatographic Determination ◽  
Gas Chromatography Mass Spectrometry ◽  
Volatile Profile ◽  
Sulphur Compounds ◽  
Physico Chemical ◽  
Acacia Honey ◽  
Value Determination

Honey composition and color depend greatly on the botanical and geographical origin. Water content, water activity and color of 50 declared acacia samples, collected from three different geographical zones of Romania, together with chromatographic determination of sugar spectrum were analyzed. A number of 79 volatile compounds from the classes of: Alcohols, aldehydes, esters, ketones, sulphur compounds, aliphatic hydrocarbons, nitrogen compounds, carboxylic acids, aromatic acids and ethers were identified by solid-phase micro-extraction and gas-chromatography mass spectrometry. The overall volatile profile and sugar spectrum of the investigated honey samples allow the differentiation of geographical origin for the acacia honey samples subjected to analysis. The statistical models of the chromatic determination, physicochemical parameters and volatile profile was optimal to characterize the honey samples and group them into three geographical origins, even they belong to the same botanical origin.

Gas Chromatographic Determination of the Plant Growth Regulator Flurprimidol in Soil and Soil-Grass Samples

1986 ◽  
Vol 69 (4) ◽  
pp. 572-575
Author(s):  
Sheldon D West ◽  
Bonnie S Rutherford
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Detection Limit ◽  
Plant Growth ◽  
Plant Growth Regulator ◽  
Chromatographic Determination ◽  
Gas Chromatography Mass Spectrometry ◽  
Electron Capture Detection ◽  
Control Samples

Abstract A method is described for the determination of flurprimidol residues in soil and soil-grass samples. Flurprimidol is extracted from the sample by refluxing with methanol-water. An aliquot is partitioned into hexane and purified by alumina B Sep-Pak column chromatography. The compound is detected and measured by gas chromatography with electron capture detection. Residue identity is confirmed by gas chromatography-mass spectrometry with detection at m/z 269.0. The detection limit is 0.01 ppm, and recoveries for control samples fortified with flurprimidol at 0.01-2.0 ppm averaged 80% for soil and 78% for soil-grass samples.

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