Pyrrolidinophenone derivatives are the group of narcotic drugs controlled in the Russian Federation. The review presents the trends of biotransformation of а-pyrrolidinovalerophenone and 3,4-methylenedioxypyrovalerone, the data about their primary metabolites is provided. Various techniques of the sample preparation of biological fluids for analytical toxicology studies for substances of the pyrrolidinophenone derivative group are discussed. The use of enzymatic hydrolysis followed by solid-phase extraction (sorption) provides low detection limits for native sub- PHARMACY ФАРМАЦИЯ stances of this group and primary metabolites using small volumes of biological fluids (0.5 and 1.0 ng/ml blood for a-pyrrolidinovalerophenone and 3,4-methylenedioxypirovalonone respectively). The main characteristics of pyrro-lidinophenone derivatives (Kovac’s retention indices in nonpolar stationary liquid phases and the main characteristic ions in the mass spectra of electron impact) are presented. They allow to identify pyrrolidinophenone derivatives and their primary metabolites in biological fluids during chromatographic-mass spectrometric screening. Analytical possibilities of an alternative variant of screening for biological fluids i.e. analysis by using current immunochemical test systems, including “biochips” are discussed. The main methods of reliable identification and quantitative determination of pyrrolidinophenone derivatives are chromatography-mass spectrometry and high-performance liquid chromatography-tandem mass spectrometry. The detection limit of 3,4-methylenedioxypyralovalone in blood by gas chromatography-mass spectrometry is 1.0 ng/ml. The ranges of the determined concentrations of the method of quantitation by gas chromatography-mass spectrometry are 2.0-2000.0 ng/ml for blood and 0.05-50.0 ng/10 mm for hair. The high-performance chromatography-tandem mass spectrometry method with a triple quadrupole in the monitoring mode of multiple molecular reactions makes it possible to achieve a nearly complete suppression of analytical background “noise” for a sample, and to obtain detection and quantification limits for 3,4-methylenedioxypy-raloperone in cadaveric blood at a level of 10.0-100.0 pg/ml and 1.0-10.0 ng/ml, respectively. One of the advantages of the high-performance chromatography-tandem mass spectrometry system is the screening possibility.
Sensitivity enhancement using a microbore column and pulsed pressure injection in the simultaneous analysis of 356 pesticide multiresidues by gas chromatography–tandem mass spectrometry
