What is Heroin
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Heroin is consider, as crude preparation of diamorphine. A semisynthetic product, obtained by acetylation of morphine, which occurs as a natural product in opium: the dried latex of certain poppy species (e.g. Papaver somniferous L.). Diamorphine is a narcotic analgesic used in the treatment of severe pain. heroin is most often related as the last grade of cocaine .In Western Europe, brown heroin (diacetylmorphine) is usually sold as the free base on the black market.Footnote1 The addition of acid, most frequently ascorbic acid or citric acid, is thus mandatory to obtain a water-soluble product usable for intravenous (IV) injection .Footnote 2 Heroin and its degradation products 6-monoacetylmorphine (MAM) and morphine are responsible for the effect on the drug consumer . This process is a metabolic pathway but can also occur during the preparation of the drug by heating.
Method of producing Heroin
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To begin ,Comparison of diacetylmorphine, 6-monoacetylmorphine, morphine, paracetamol and caffeine concentrations were performed in the non-processed material, after processing according to the standard and to the alternative preparation methods, using liquid chromatography coupled to quadrupole time of flight mass spectrometry followed by statistical evaluation of the results ,from the liquid is heated and turns to powder .
Brown heroin is the only form of heroin available at the Luxembourgish illegal drug market. A total of 30 independent samples received in 2019 from seizures of the Luxembourgish police or customs office have been randomly selected for analysis.
Chemicals and materials
Diacetylmorphine (1 mg/mL, Lot# 687,046), 6-monoacetylmorphine (MAM, 1 mg/mL, Lot# 39,582), morphine (1 mg/mL, Lot# 88,283), paracetamol (1 mg/mL, Lot# 158,876) and caffeine (1 mg/mL, Lot# 980,098) were obtained from LGC Standards (Molsheim, France).
UPLC grade water with 0.1% formic acid (solvent A) and UPLC grade acetonitrile with 0.1% formic acid (solvent B) were purchased from Fisher Chemical (Waltham, MA, USA). Aluminum cookers (Apothicom Stericup, Chirana T. Injecta), ascorbic acid (Vitamin C, 100 mg, Chirana T. Injecta) and physiological saline solution (0.9% NaCl in water, Physio Flexo, 2 mL) were gifted from Abrigado (Luxembourg City).
All samples were extensively homogenized before cooking. The standard preparation method consisted in mixing 100 mg of heroin powder with 50 mg of ascorbic acid in the aluminium cup, prior the addition of 1 mL of saline solution. A gas lighter was used to heat uniformly the aluminium cup until complete dissolution of the solid material. This step took 15–60 s.
The “Turkish” preparation method consisted in mixing 100 mg of heroin powder with 50 mg of ascorbic acid in the aluminum cooker without addition of saline solution. After heating until liquefaction of the starting material (15–30 s), 1 mL of saline solution was added. A second heating step (30–60 s) was applied to obtain the final homogenous solution.
Independently of the preparation method, the final solutions were allowed to cool down to room temperature (> 2 min) before qualitative and quantitative analyses.
The analyses were performed using a LC-based high-resolution mass spectrometer in order to prevent the presence of artefacts that may result from the high temperature required in GC-based analyses (i.e., trans-acetylation).Footnote12
Screening for other compounds than diacetylmorphine, MAM, morphine, paracetamol and caffeine were performed on a G6550A ifunnel Q-ToF LC–MS system (Agilent, Waldbronn, Germany) equipped with a 1290 Infinity HPLC system. The system was operated using an Agilent MassHunter Workstation.
Chromatographic separation was achieved on a C18 column (Acquity UPLC BEH C18 Column, 130 Å, 1.7 µm, 1 mm × 50 mm). The elution was carried out by applying a mixture of solvents A and B. The compounds of interest were eluted using a linear gradient from 2 to 95% solvent B over 7 min at a flow rate of 0.3 mL/min and an oven temperature of 60 °C. The injection volume was 5 µL. The ESI interface was operated in positive ionization mode. The MS acquisition was performed in auto MS/MS mode (top 5) from 70 to 1700 m/z in MS and 50 to 1700 m/z in MS/MS. Acquisition rate was 3 spectra/s, and collision energy was determined using the following equation: 6 * m/z/100 + 4.Footnote13 Precursor selection was performed using an absolute threshold of 200 counts, a relative threshold of 0.01% active exclusion after 1 spectrum released after 0.15 min. Reference masses were 121.050873 and 922.009798 m/z. Identification was realized using exact m/z, retention time databases and MS/MS database (High Res NPSFootnote14). The corroboration of compounds identity was performed with mass tolerance of ± 0.005 Da and ± 0.05 Da for precursor and fragment ions, respectively, and retention times at ± 0.5 min, if known.
The same analytical system as for the qualitative screening was used for quantitative analyses. The compounds were eluted using a gradient from 0 to 100% solvent B over 26 min. The flow rate was 0.3 mL/min at 40 °C. The test solutions were diluted 100 times in 1000 µL of a mixture of solvent A and solvent B (9/1 V/V); 5 µL were injected into the LC-Q-ToF system. The MS acquisition was realized in positive MS mode from 50 to 500 m/z with an acquisition rate of 3 spectra/s and no collision energy was applied. Reference masses were the same as for the qualitative analysis. The area under the curve (AUC) was used to quantify each compound of interest. The quantification was performed using a four-point external calibration curve (0, 0.05, 0.10 and 0.50 mg/L).
In order to access the variability of the “Turkish” cooking method, a repeatability test was carried out by analyses of 12 aliquots of the same heroin sample. The relative standard deviation (RSD) was calculated, for each compound of interest, using the following formula:
with s: standard deviation and x: mean concentration.
To evaluate the concentration changes of a compound of interest depending on the cooking methods, the P-value of the two-tailed t-test was calculated. The significance level was set to 0.05 (p > 0.05: no significant difference).
Heroin lab result test
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These two preparation methods ,had in common a diminution of diacetylmorphine . If compared to the starting material , significantly more 6-monoacetylmorphine was produced using the “Turkish” preparation method as compared to the standard method.This is considered the lab result .
Qualitative and quantitative analyses of the 30 heroin samples were carried out on the raw material (prior to any cooking step), and after going through both the standard and the “Turkish” cooking methods.
Prior to cooking, qualitative screening was performed on all samples in order to access the sample compositions. All samples contained diacetylmorphine, MAM, paracetamol and caffeine. Morphine was detected in five out of the 30 samples. No psychoactive substances other than diacetylmorphine, MAM and morphine were detected (i.e., cocaine, fentanyls, new psychoactive substances, etc.) and no adulterants other than paracetamol and caffeine either (i.e., grisoefulvine and strychnine). Furthermore, none of the diacetylmorphine degradation products described by Cook and Brine were detected in the samples prior or after any type of cooking5.
The compounds of interest were quantified in the samples prior to cooking. The results (Table 1) are in concordance with data published by the EMCDDA.Footnote15 In particular, diacetylmorphine concentration range was from 3.5 to 46.5%, mean concentration was 18.9% and median concentration was 20.3%. MAM and morphine concentrations were low, often < LOQ. 1kg Heroin