Lab-made solid phase microextraction phases for off line extraction and direct mass spectrometry analysis: Evaluating the extraction parameters.

The analyses of drugs and metabolites in complex matrices have been widely studied in recent years. However, due to high levels endogenous compounds and matrix complexity, these analyses require a sample pre-treatment step. To this aim, two lab-made extractive phases were integrated to probe electrospray ionization mass spectrometry (PESI-MS) technique for direct analysis of illicit drugs in biological fluids and phorbol esters in Jatropha curcas extract. The polypyrrole (PPy) phase was electropolymerized onto a platinum wire surface by cyclic voltammetry. The molecularly imprinted polymer (MIP) was synthesized and adhered onto a stainless-steel needle with epoxy resin. The PPy-PESI-MS method showed to be linear in a concentration range from 1 to 500 µg L-1, with accuracy values between -2.1 and 14%, and precision values between 0.8 and 10.8%. The MIP-PESI-MS method showed to be linear in a concentration range from 0.9 to 30 mg L-1, with accuracy values between -1.6 and -15.3%, and precision values between 4.1 and 13.5%.

Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour - Determination by high-performance thin-layer chromatography-fluorescence detection.

Ergot alkaloids are generally determined by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD) or mass selective detection, analyzing the individual compounds. However, fast and easy screening methods for the determination of the total ergot alkaloid content are more suitable, since for monitoring only the sum of the alkaloids is relevant. The herein presented screening uses lysergic acid amide (LSA) as chemical marker, formed from ergopeptine alkaloids, and ergometrine for the determination of the total ergot alkaloids in rye with high-performance thin-layer chromatography-fluorescence detection (HPTLC-FLD). An ammonium acetate buffered extraction step was followed by liquid-liquid partition for clean-up before the ergopeptine alkaloids were selectively transformed to LSA and analyzed by HPTLC-FLD on silica gel with isopropyl acetate/methanol/water/25% ammonium hydroxide solution (80:10:3.8:1.1, v/v/v/v) as the mobile phase. The enhanced native fluorescence of LSA and unaffected ergometrine was used for quantitation without any interfering matrix. Limits of detection and quantitation were 8 and 26µg LSA/kg rye, which enables the determination of the total ergot alkaloids far below the applied quality criterion limit for rye. Close to 100% recoveries for different rye flours at relevant spiking levels were obtained. Thus, reliable results were guaranteed, and the fast and efficient screening for the total ergot alkaloids in rye offers a rapid alternative to the HPLC analysis of the individual compounds.

Application of micellar electrokinetic capillary chromatography to the analysis of illicit drug seizures.

The application of micellar electrokinetic capillary chromatography (MECC) to the analysis of illicit drug seizures is presented. Areas investigated include general screening and qualitative and, in some instances, quantitative analysis of various drugs, including heroin, opium, cocaine, amphetamines, LSD and anabolic steroids. Due to its high efficiency, high selectivity and general applicability, MECC is well suited for forensic drug analyses.

The detection and characterization of controlled drugs imported into the United Kingdom.

The Laboratory of the Government Chemist examines most of the drugs that have been seized at the point of entry into the United Kingdom of Great Britain and Northern Ireland and has developed analytical methods for their rapid identification in the field and for more exact analysis and quantitation in the Laboratory. These methods are described for the major types of drugs encountered. Many seizures are examined in greater detail in order to compare samples and to correlate origin with physical and chemical appearance. Information on the procedures necessary to undertake this aspect of work is also presented.

Role played by narcotics laboratories in the campaign against drug abuse and drug trafficking: a view from a developing country.

The narcotics laboratory at the national level identifies drugs for abuse and their accompanying substances in suspected samples, determines the purity and the possible origin of illicit drugs, carries out drug-related research, particularly on new sources of drugs liable to abuse, and, when required by the police or courts of law, provides supportive expertise in drug trafficking cases. Precaution must be taken to ensure that samples to be examined are representative. The university is a particularly appropriate setting for the location of a narcotics laboratory, especially if such a laboratory carries out complex work requiring assistance from other professional disciplines. Before new laboratory equipment is purchased, a careful study of requirements and financial resources should be made to ensure economical and optimum utilization of such equipment. In some situations the use of simple techniques, such as thin-layer chromatography, can be sufficient, while in others more sophisticated techniques may be required. Appropriate training of personnel is of particular importance for the effective functioning of a narcotics laboratory. The laboratory of the Department of Toxicology and Forensic Chemistry, University of Buenos Aires, provides for the training of personnel at three levels: The first level consists of basic training, which includes the use of kits for rapid identification of drugs in field conditions, for personnel from the police, gendarmerie, prefecture, customs and other agencies which deal with drug problems, but which have no previous skills in laboratory techniques; The second level is provided for professional laboratory personnel and usually lasts six months; The third level consists of two years' postgraduate university training for students who are expected to carry out complex laboratory work; an additional year is provided for trainees who are expected to assume responsibility in a laboratory unit.

Forensic aspects of high-pressure liquid chromatography.

This paper reviews the applications of high-pressure liquid chromatography (HPLC) to forensic problems, and discusses some of the developments that have taken place in the use of the technique in the Metropolitan Police Laboratory. Preparation of octadecyltrichlorosilane-modified silica is described and some of the chromatographic characteristics of this material are investigated. Applications of HPLC to the analysis of cannabis, opium alkaloids, amphetamine-related materials, LSD and polynuclear hydrocarbons are described.