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COMPONENT ANALYSIS OF ILLICIT
HEROIN SAMPLES BY GC-MS METHOD
MIHAELA GHEORGHE1*, DAN BĂLĂLĂU2, MIHAELA ILIE2,
DANIELA-LUIZA BACONI2, ANNE-MARIE CIOBANU3
1
Criminalistics 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.
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


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
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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
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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.
Figure 1. Chromatogram of sample X and mass spectrum of caffeine
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Figure 2. Chromatogram of sample Z
Figure 3. Chromatogram of sample U
Figure 4. Chromatogram of sample V
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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.
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