Quantitative analysis heroin

There are two types of analysis qualitative and quantitative. Qualitative analysis determines which chemical is present, while quantitative analysis determines the concentration of a chemical. Concentration means an amount of chemical per unit of sample, for example, 100 micrograms (pg) of morphine per liter (L) of blood (100 pg/L) or the amount of pure chemical per weight of material, such as 1 gram of heroin per 10 grams of white powder. 

Rook EJ, Hillebrand MJX, Rosing H, van Ree J, Beijnen JH (2005) The quantitative analysis of heroin, methadone, and their metabolites and the simultaneous detection of cocaine, ace-tylcodeine and their metabolites in human plasma by high-performance liquid chromatography coupled with tandem mass spectrometry. J Chromatogr B 824 213-221... 

Quantitative analysis showed that the concentrations of heroin and quinine in all exhibits were approximately equal. The determination of the relative concentrations of heroin impurities are given in Table IV, and were all similar. Expert testimony was given that all five exhibits originated from a common source and this testimony was an integral part of the prosecution s case establishing a conspiracy. 

Gough and Baker studied a number of conventional and modified stationary phases in order to find the best one for quantitative gas chromatography of heroin and structurally related compounds. Silanized 0V-210 was found to be the most suitable for the separation of heroin, codeine, acetylcodeine, morphine and 6-0-monoacetylmorphine. It gave the best reproducibility of retention times and less losses of the compounds by adsorption. For quantitative analysis 2.8 m by 4 mm I.D. glass columns and Diatomite CLQ, 80-100 mesh, as solid support were used at a column temperature of 225°C. Despite the fact that some of the compounds, particularly morphine, suffered adsorption losses during gas chromatography, these losses were reproducible, and satisfactory quantitative data could be obtained, as shown in Table 14.19. 

Petroff and co-workers reported a quantitative analysis of the H NMR spectra of six CSF samples from three patients. TTiese included a 34-year-otd man presenting with seizures several hours after injecting heroin and cocaine while intoxicated with alcohol, and a 7-month-old girl who presented as a febrile, cyanotic hypotensive in a coma. The H NMR spectrum of the CSF of the drug overdose victim showed clear and abnormally elevated signals for citrate, myo-inositol, creatinine/creatine and lactate. 

Hays, P.A. Lurie, I.S. Quantitative analysis of adulterants in illicit heroin samples via reversed phase HPLC. J.Liq.Chromatogr., 1991, 14, 3513—3517 [also acetylcodeine, acetylmorphine, aspirin, ben-zocaine, caffeine, chloroquine, diamorphine, diazepam, diphenhydramine, dip3rrone, lidocaine, meth-aqualone, monoacetylmorphine, morphine, nicotinamide, noscapine, papaverine, phenacetin, pheno-barbital, phenolphthalein, N-phenyl-2-naphthylamine, salicylic acid, strychnine]... 

Lurie, I.S. McGuiness, K. The quantitation of heroin and selected basic impurities via reversed phase HPLC. II. The analysis of adulterated samples. J.Liq.Chromatogn, 1987, 10, 2189-2204 [UV detection electrochemical detection also acetaminophen, acetylcodeine, acetylmorphine, acetylprocaine, aminopyrene, amitriptyline, antipyrine, aspirin, barhital, benztropine, caffeine, coceiine, diamor-phine, diazepam, diphenhydramine, dipsrone, ephedrine, ethylmorphine, lidocaine, meconin, meth-amphetamine, methap3rrilene, methaqualone, morphine, nalorphine, niacinamide, noscapine, papaverine, phenacetin, phenmetrazine, phenobarbital, phenolphthalein, procaine, propanophenone, propoxyphene, pyrilamine, quinidine, quinine, salicylamide, saliqrlic acid, secobarbital, strychnine, tartaric acid, tetracaine, thebaine, tripelennamine, tropacocaine, vitamin B3, vitamin B5]... 

For quantitative analysis, Bertol et al. (1989) found that a programmable temperature vaporizer inlet increased the accuracy of the analysis since it eliminated discrimination problems when analyzing compounds with a large range of molecular weights. With this method it was possible to increase the accuracy of the quantification of heroin, monacetylmorphine, acetylcodeine, papaverine, and narcotine commonly found in street samples of heroin. 

See also Amphetamines. Blood and Plasma. Clinical Analysis Glucose. Fluorescence Quantitative Analysis. Forensic Sciences Blood Analysis Gunshot Residues Systematic Drug Identification. Heroin. Proteins Physiological Samples. 

Many pharmaceuticals can be studied successMly using this technique, for example 1 mg of heroin in potassium bromide (Fig. 10). It is possible to monitor the concentration of heroin in a potassium bromide sample once a calibration graph has been prepared. The DRIFTS technique can be applied to quantitative analysis. 

Lerner and Mills (JjO reported the presence of 0 -monoacetyl-morphine as a common constituent in heroin and suggested that the ratio of heroin to monoacetylmorphine would not change during adulteration. Others have dealt primarily with the identification of the adulterants present, either other drug substances or sugars (6,7). Grooms (j3) and Miller (9) have attempted to include the analysis of adulterants with the presence of monoacetylmorphine. In each of these cases, the resolution of the various components was insufficient to provide good quantitative data. 

Work is continuing on the analysis of heroin exhibits to develop a larger data base. Work is also continuing on more quantitative methods for adulterated heroin samples. 

In most forensic laboratories, the largest amount of HPLC time is taken up with the analyses of drugs of abuse (often called street drugs) i.e. amphetamines, heroin, cocaine, LSD, etc. The purpose of any drug s HPLC analysis is to confirm the identity of drug and provide a quantitative result. With the exception of LSD, relatively large quantities of a drug sample are usually available and UV detection is preferred since it offers... 

The analysis of heroin samples gives rise to a different set of problems. Heroin contains a mixture of opiate alkaloids and one of these, diamor-phine (diacetylmorphine), is the controlled drug which has to be determined quantitatively. The other major opiates present in heroin can... 

The determination of the heroin metabolites morphine, morphine-6-glucuronide (M6G), morphine-3-glucuronide (M3G), and 6-monoacetyhnorphine (6-MAM) in body fluids is an important application of LC-MS in the toxicology laboratory. In some cases, codeine and codeine-6-glucuronide are determined as well. Several quantitative methods have been reported. However, only a few deal with forensic toxicology, performing the analysis in urine, serum, vitreous humour [79], and autopsy whole blood [79-80]. 

The opium alkaloids have engaged the interest of scientists since the isolation of morphine by Sertlirner in 1806. The Isolation, characterization and quantification of these alkaloids have been a continuing challenge. Gas chromatography of opium alkaloids has been performed i.a. for the analysis of the alkaloids present in the crude drug itself, especially for the quantitative determination of morphine, as well as for the analysis of opium alkaloids, mainly morphine - and heroin - in biological materials. Most studies have so far been carried out with packed columns, only a limited number with capillary columns. 

Klein applied gas chromatography. 3-0-acetylmorphine results from an incomplete esterification of morphine with acetic anhydride and the amount may be of value for forensic purposes. Because of the very small amounts present in heroin, the compound was derivatized with hepta-fluorobutyric anhydride and gas chromatographed with a Ni electron capture detector on a 3 1 OV-17 on Gas Chrom Q packed column at 230°C using chlorpromazine as an internal standard. The heptafluorobutyric anhydride derivatives were extracted quantitatively from the reaction mixture with light petroleum and were stable for several hours in this solvent. However, it was recommended that upon formation, the analysis should be completed without delay. The analysis was carried out with 1-10 mg heroin samples and the amount of 3-0-acetylmorphine varied from 0.1 to 2 %, acetylcodeine from 3 to 15, morphine and codeine from 0.01 to 0.5. ... 

Van Vendeloo et al. developed a gas chromatographic method for fingerprint analysis of illicit heroin samples, capable of detecting the main components acetyl codeine, caffeine, codeine, heroin, 6-0-monoacetylmorphine, morphine and quinine in one run in 25 min. Heroin, morphine, codeine and caffeine could be quantified directly, 6-0-monoacetylmorphine and acetylcodeine were not fully separated. Quantitation of the latter two required acetylation of 6-0-monoacetylmorphine to heroin. A packed column of 1 % OV-1 on Chromosorb G HP was used... 

Shui-Tse Chow stated that the only physical method offering the necessary identification selectivity with quantitative capability for the gas chromatographic analysis of heroin in illicit samples is selected 1on monitoring (SIM) mass spectrometry. Deuterated heroin and the ions m/e 369 and 327 for heroin and 375 and 331 of deuterated heroin were used as internal standards and the ions m/e 369 and 327 were quantified and calculated as heroin. The calibration curves for both m/e 375/369 and m/e 331/327 were linear within the concentrations studied. The gas chromatographic analysis was qarried out on a 1.8 m by 6.35 imi O.D. glass column packed with 3 % OV-17 on Chromosorb W HP, 100,120 mesh, at a column temperature of 270°C. For GC-MS 1.8 m by 6.35 mm O.D. glass columns were used, packed with 3 OV-1 on Chromosorb W HP, 100-120 mesh, and a column temperature of 250°C. The results obtained are summarized in Table 14.20. 

Whereas detection limits for heroin with conventional FID are reported as 0.05 mg/ml in blood from illicit preparations, a nitrogen specific detector can quantitate levels of 100 ng/ml - and detection limits can be as low as 20 ng/ml according to Smith and Cole3 3. They determined heroin and its metabolite 6-0-acetylmorphine in blood after extraction and deriva-tization to its trifluoroacetate, to prevent adsorption during the gas chromatographic analysis when the free hydroxyl group was present. Ethylmorphine, derivatized in the same way was used as an internal standard. 

Raman spectra of drugs are fuU of information and are unique to each substance. Very similar chemicals, e. g. amphetamine x HCl and amphetamine sulfate or heroin and morphine, yield very different spectra. Usually such samples consist of many constituents, hence multivariate analysis (cf. Chapter 13) should be used to obtain quantitative models of drug concentrations in solid mixtures. The abihty to correctly identify unknowns also depends upon the availabihty of high-quahty reference spectra. 

Early chemical profiling attempted to establish batch links among illicit drug seizures by comparative studies, based on both qualitative and quantitative information, although success in achieving this has been varied. Such studies have been applied to link heroin and cocaine samples to common origins, based on the concentration of the organic impurities present. Isotopic analysis of impurities and intermediates has been employed in the comparison of seized heroin, methamphetamine, and ecstasy samples. X-ray diffraction and NMR spectroscopy (both and have been used to... 

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