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Component analysis of illicit heroin samples by gc-ms method


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FARMACIA, 2008, Vol.LVI, 5



COMPONENT ANALYSIS OF ILLICIT HEROIN SAMPLES BY GC-MS METHOD
MIHAELA GHEORGHE1*, DAN BĂLĂLĂU2, MIHAELA ILIE2, DANIELA-LUIZA BACONI2, ANNE-MARIE CIOBANU3

1Criminalistics Research Institute of the Romanian Police General Inspectorate, 13-15 Ştefan cel Mare Str., Bucharest, Romania

2”Carol Davila” University of Medicine and Pharmacy, Faculty of Pharmacy, Toxicology Department, 6 Traian Vuia Str., Bucharest, Romania

3”Carol Davila” University of Medicine and Pharmacy, Faculty of Pharmacy, Medicines Control Department, 6 Traian Vuia Str., Bucharest, Romania

*corresponding author: mihag72@yahoo.com


Abstract

Opiates are narcotics having a high potential for addiction, with a fast development of tolerance and a severe withdrawal syndrome at the cessation of the administration.

Heroin, a highly addictive drug, is the most abused of the of the opiates; its abuse has repercussions that extend far beyond the individual user.

Illicitly produced heroin is commonly adulterated with other drugs or substances to increase bulk. The component analysis of street heroin samples is important for legal purposes, and often the sensitivity and the reliable of the method choosed for the identification are crucial.

The paper presents the component analyses of seized illicit heroin by a GC- MS method. The main components in illicit heroin products such as heroin, acetylcodeine, and noscapine were identified in the most samples; the organic adulterants such as caffeine and phenobarbital were also detected.
Rezumat

Opiaceele reprezintă o clasă de narcotice cu un potenţial ridicat de inducere a dependenţei, caracterizată prin dezvoltarea rapidă a toleranţei şi declanşarea unui sindrom de abstinenţă grav la întreruperea administrării.

Heroina, având un potenţial adictiv ridicat, este drogul cel mai frecvent utilizat dintre opiacee; abuzul de heroină are consecinţe care depăşesc cu mult nivelul individual.

Heroina produsă ilicit este falsificată în mod obişnuit cu alte droguri sau substanţe comune pentru a creşte cantitatea. Analiza componentelor probelor de heroină de stradă este importantă pentru scopuri legislative şi adesea sensibilitatea şi gradul de certitudine ale metodei alese pentru identificare sunt cruciale.

Lucrarea prezintă analiza calitativă prin metodă GC-MS a unor probe de heroină confiscate de pe piaţa ilicită. In majoritatea acestor probe componentele principale identificate au fost heroina, acetilcodeina şi noscapina, însă au fost detectaţi de asemenea, adulteranţi precum cafeina şi fenobarbitalul.


  • illicit drugs

  • heroin

  • GC-MS


INTRODUCTION

Heroin is an illegal, highly addictive drug. It is both the most abused and the most rapidly acting of the opiates.

Heroin is processed from morphine, a natural alkaloid occurring in opium.

Usually, street heroin is “cut” with other drugs or with substances such as caffeine, quinine, strychnine, phenobarbital, sugar, starch, powdered milk etc [1].

Because heroin abusers do not know the actual strength of the drug or its true contents, they are at risk of overdose or death.

The identification of the components can give valuable information on the drug provenance.

Several techniques have been used to analyse the components in street heroin samples, with GC-MS being by far the most widely used analytical technique [2- 5].

The GC-MS is considered a "gold standard" for forensic substance identification, as it is used to perform a specific test, which positively identifies the actual presence of a particular substance in a given sample.

The paper presents the results obtained at the analysis of four confiscated heroine drug samples in an attempt to establish a method for the best separation and identification of the compounds that can be found in illegal drugs.

MATERIALS AND METHODS

Substances:


  • four seized illicit drug samples, denoted X, Z, U, V

  • methanol HPLC grade (Sigma)

Instrumentation:

    • GC-MS Fisons Instrument 8060 with mass spectrometer Trio 1000

    • VF1ms cappilary column (30 m x 0,32 mm I.D., 0,25 μm film thickness)

    • Wiley 6 mass spectra library



Chromatographic conditions:

  • temperature program: the initial temperature was 50°C, held for 1 minute, programmed to 270°C at 10°C/min, and held for 10 minutes

  • injection port temperature: 270°C

  • transfer line temperature: 250°C

  • carrier gas: helium at flow rate of 2 mL/min

  • scanning range: 50-500 u.a.m.

  • ions monitored (m/z):

- caffeine: 194, 109, 55, 67, 82, 195, 42, 110

- codeine: 299, 42, 162, 124, 229, 59, 300, 69

- phenobarbital: 204, 117, 146, 161, 77, 103, 115, 118

- heroin: 327, 43, 369, 268, 310, 42, 215, 204



Sample preparation

The drug samples (10-6 g) were dissolved in methanol, and the solutions were injected in GC-MS instrument.


RESULTS AND DISCUSSION

In the chromatogram of X sample (Figure 1), five peaks are noticed, at the following scans: 789, 1017, 1135, 1164, and 1234.

For the peak at the scan 789, the mass spectrum indicates the presence of caffeine (m/z: 55, 67, 82, 109, 194, and the reverse fit factor of 977, Figure 1).

At scan 1017 phenobarbital was detected: the mass spectrum obtained with the reverse fit factor of 927 has as principal ions (m/z): 77, 117, 146, 161, 204.

For the peak at the scan 1135, the mass spectrum indicates the presence of codeine (m/z: 124, 162, 229, 299, and the reverse fit factor of 879).

The mass spectrum for the peak at scan 1164, obtained with a reverse fit factor of 789 indicates the presence of acethylcodeine (m/z: 59, 70, 81, 282, 341). Acethylcodeine is usually detected in the heroin ilicit samples, as an impurity coming from the manufacturing process.

The peak at scan 1234 belongs to heroin (m/z ions in the mass spectrum: 268, 310, 327, 369, and the reverse fit factor of 856).

The chromatogram for Z sample shows three peaks, at scan 1133, 1214, and 1695 (Figure 2); the mass spectra obtained for the above mentioned peaks certify the presence of acethylcodeine (at scan 1133), heroin (at scan 1214), and noscapine (at scan 1695). Noscapine is frequently cited in street heroin, coming from opium, the raw material for the production of heroin.

The GC-MS analysis of sample U (the chromatogram presented in the Figure 3) led to detection of acethylcodeine (at scan 1137) and heroin (at scan 1231); the obtained mass spectra had the reverse fit factors of 853 and 806, respectively.

In the sample denoted V, acethylcodeine and heroin were also identified (Figure 4) at scan 1135 and 1208, respectively.




frame1
Figure 1. Chromatogram of sample X and mass spectrum of caffeine
frame2

Figure 2. Chromatogram of sample Z
frame3

CONCLUSIONS

GC-MS method gives the possibility of a sure identification of the components in the illicit heroin samples. Our results confirm the presence of heroin, acetylcodeine, and noscapine in street heroine samples; the common adulterants such as caffeine and phenobarbital were also detected.


REFERENCES

  1. Baconi D., Toxicomanii, note de curs, Editura Tehnoplast Company S.R.L., Bucureşti, 2005, 79, 90

  2. Brenneisen R., Hasler F., GC/MS determination of pyrolysis products from diacetylmorphine and adulterants of street heroin samples, J Forensic Sci., 2002, 47(4):885-888

  3. *** Clarke’s Analysis of Drugs and Poisons in Pharmaceuticals, Body Fluids and Postmortem Material – Eds. Moffat A.C., Osselton M.D., Widdop B., Galichet L.Y., third edition, The Pharmaceutical Press, London, Chicago, 2004, 37 - 52

  4. Klemenc S., Noscapine as an adulterant in illicit heroin samples, Forensic Sci Int., 2000, 108(1), 45-49

  5. Zhang D., Shi X., Yuan Z., Ju H., Component analysis of illicit heroin samples with GC/MS and its application in source identification, J Forensic Sci., 2004, 49(1), 81-86





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