Thin Layer Chromatographic Separation of Diacetylmorphine (Heroin) and Its Excipients: an Experimental Study

Research Article J Forensic Sci & Criminal Inves Volume - 8 Issue 3 - April 2018 Copyright © All rights are reserved by Mahesh Chand Meena DOI: 10.19080/JFSCI.2018.08.555736 Thin Layer Chromatographic Separation of Diacetylmorphine (Heroin) and Its Excipients: An Experimental Study Saloni Chadha1, Deepti Bhargava2, Mahesh Chand Meena3* and VB Ramteke4 1Tutor, Department of Forensic Medicine & Toxicology, Dr BSA Medical College & Hospital, Indraprastha University, India 2Senior Scientific Officer-II, Chemistry Division, Central Forensic Science Laboratory, India 3MD (Forensic Medicine), Assistant Professor, Department of Forensic Medicine & Toxicology, Dr BSA Medical College & Hospital, Indraprastha University, India 4SSO-I & HOD, Chemistry Division, Central Forensic Science Laboratory, India Submission: April 04, 2018; Published: April 17, 2018 *Corresponding author: Dr Mahesh Chand Meena, MD (Forensic Medicine), Assistant Professor, Department of Forensic Medicine & Toxicology, Dr BSA Medical College & Hospital, Indraprastha University, Rohini, Delhi, India, Email: Abstract Background Heroin is a well-known drug of abuse that is usually administered intravenously. However, smoking heroin has gained popularity samplesin many wereparts receivedof the world in sealed since transparent it was first plasticdescribed containers in Shanghai for qualitative in the 1920s. analysis Material of heroin and method- and its excipients. A total of 6Result-Out exhibits were of 16 examined systems, 11in systemslaboratory, are New capable Delhi of for resolving research opium work andand itsthe alkaloids, physical appearances9 systems are were capable noted of for resolving the samples opium as alkaloids a part of inthe illicit preliminary heroin and examination. 8 systems The are capable of resolving opium alkaloids and adulterants in illicit heroin. Conclusion In our study the best solvent systems are Ethyl acetate: benzene: acetonitrile: ammonia (25:30:40:5) and Toluene: acetone: ethanol: ammonia (20:20:3:1) for separation of opium alkaloids and adulterants. Keywords : Heroin; Thin layer chromatography; Opium alkaloids; Adulterants. Abbreviations : TLC: Thin Layer Chromatography; DAM: Diacetylmorphine; MAM: Mono Acetyl Morphine. Introduction Historically, and more recently it has been a common practice that illicit drugs such as heroin typically contain other from it some gratification for his desire [3]. Nearly every small approximately equal amount of lactose or powdered sugar. As disturbances in addition to the purported active ingredients that peddler who resells heroin first mixes his supply with at least an his heroin is usually highly adulterated and diluted even before can have serious adverse health consequences or even cause premature death [1]. Heroin is a well-known drug of abuse that is usually administered intravenously. However, smoking heroin he gets it, it frequently reaches the final user containing no more little as one per cent [4]. An illicit heroin sample may contain has gained popularity in many parts of the world since it was than five per cent of the actual alkaloid, or even sometimes as a number of natural and synthetic opiate alkaloids as well as adulterants and diluents. Additional substances may be added called ‘‘chasing the dragon’’ addicts typically inhale heroin first described in Shanghai in the 1920s [2]. In a procedure to bulk, dilute, complement or enhance the effects of the drug fumes resulting from heating heroin powder on aluminum foil or mimic the effects of illicit drugs or that will facilitate the with a cigarette lighter until it melts and evaporates. Heroin is administration of the illicit drug such as caffeine in heroin and in cocaine to facilitate smoking. Diluents are chemicals smoking, subcutaneous injection and intravenous injection [3]. administered in several ways. These include sniffing or snorting, The great advantage of heroin, from the point of view of lactose, mannitol, corn starch, dextrose, sucrose, sodium added to controlled substances that are used as fillers like bicarbonate, sodium carbonate, magnesium sulphate, sodium dilution with other substances, while still the addict obtains f chloride, caffeine, etc [4]. Adulterants commonly encountered illicit traffickers, is that it seems capable of almost unlimited J Forensic Sci & Criminal Inves 8(3): JFSCI.MS.ID.555736 (2018) 001 Journal of Forensic Sciences & Criminal Investigation in heroin include quinine, procaine, acetaminophen, caffeine, Methanol, Chloroform, Diethyl ether, Diethyl amine, Ethyl diphenhydramine, aspirin, Phenobarbital, strychnine, diazepam, acetate, Acetonitrile, n-butanol( HPLC Grade, purchased from methaqualone and lidocaine and quinine, procaine [4]. Merck & Spectrochem) Mono-acetyl morphine and morphine remain from imperfect Method for processing TLC plates acetylation as consequences of impurity of manufacture. a) The TLC tanks were pre-equilibrated with the desired Codeine, papaverine and meconic acid prove that their presence solvent system one hour before use, and were made up to is a result of crude process being used not only to manufacture 50ml, thoroughly mixed and then left for equilibration. of narcotic and psychotropic substance requires the use of b) The individual standards were dissolved in methanol but for purification of heroin as well [4]. Chemical examination to a concentration of 1 mg/ml. The mixture was prepared by examination, we switch on to instrumental techniques with mixing equal volumes of the standards. instruments as confirmatory techniques. After preliminary thin layer chromatography (TLC) being the most convenient c) The spotting line of the TLC plate was kept 1.5cm from the bottom of the plate. HPTLC which minimizes the chances of human error caused and rapid method of separation & identification followed by by evaluating TLC. The use of sophisticated instruments like d) A spotting volume of approx. 2 µl was applied 1.5cm from the edge of the plate to overcome edge effect and 2mm and are the last resort of identifying compounds in an unknown in diameter approximately. The spreading of spots was GC, GC-MS, and UV permits high accuracy and efficient results sample. In examining a “Heroin” sample the primary necessity restricted to the maximum. is to identify the diacetylmorphine with complete certainty, or to identify the narcotic substances present [3]. The present 1cm. study was to determine best solvent systems for the separation e) The distance between subsequent spots was fixed to of diacetylmorphine (Heroin) along with other opium alkaloids f) The plate was allowed to run for a distance of 10cm and adulterants present in samples of illicit heroin by using from the starting line of the plate. chromatographic techniques. g) After the complete run, the plates were taken out of the Material and Methods chamber and air dried. h) Developed plates were visualized under UV light and Delhi for research work and the physical appearances were noted spraying with chromogenic reagents A total of 6 exhibits were examined in the laboratory, New for the samples as a part of the preliminary examination. The TLC systems samples were received in sealed transparent plastic containers for qualitative analysis of heroin and its excipients. The samples Table 1: listing the solvent systems to be evaluated for thin layer chromatograph. were weighed. The weight of each sample was 10gm approx. Each of approximately 0.5gm of each sample was taken for analysis in S . No. TLC System References test tubes which were marked with sample number. Pre-coated Cyclohexane: benzene: diethyl amine plates were obtained from Merck (20 x 20 cm aluminum backed; I 6 (70:25:10)- silica gel 60 GF 254; 0.2 mm layer thickness). Developed plates Ethyl acetate: methanol: II 7 were visualized under UV at 254nm and with spray reagents ammonia(85:10:5)- (Dragendorff reagent, Iodoplatinate reagent, Marquis reagent, Toluene: acetone: ethanol: ammonia III 8 Froehde reagent, Liebermann’s reagent & Potassium Ferro (20:20:3:1) cyanide +ferric chloride). Cyclohexane: chloroform: diethyl IV 8 amine(70:25:10) The individual standards were dissolved in methanol to a concentration of 1 mg/ml. The mixture was prepared by mixing V Benzene: acetone: ammonia(50:50:2) 8 equal volumes of the standards. A spotting volume of 2 µl was VI Benzene: ethanol(4:1) 9 applied. The TLC tanks were pre-equilibrated with the solvent Ethyl acetate: benzene: acetonitrile: VII 10 system 15 minutes before use. Spray reagents were prepared ammonia (25:30:40:5) according to E. C. G. Clarke [5-17]. Cyclohexane: toluene: diethyl amine VIII 8 (70:25:10) - opium, heroin, mono acetyl morphine, Standard Drugs IX Benzene: methanol (4:1) 11 narcotine, papaverine, thebaine, codeine, acetyl codeine, Diethyl ether: acetone: diethyl amine X 12 lidocaine, caffeine, diphenhydramine, nitrazepam, diazepam, (85:8:7)- paracetamol, methadone, dexmetorphan, alprazolam Diethyl ether (water saturated): acetone: XI 13 Chemicals- Cyclohexane, Benzene, Diethyl amine, Ethyl diethyl amine(85:8:7) acetate, methanol, Ammonia, Acetone, Toluene, Ethanol, XII n-butanol: acetic acid: water (35:3:10) 14 How to cite this article: JerrSaloni C, Deepti B, Mahesh C M, VB Ramteke. Thin Layer Chromatographic Separation of Diacetylmorphine (Heroin) and 002 Its Excipients: An Experimental Study. J Forensic Sci & Criminal Invest. 2018; 8(3): 555736. DOI: 10.19080/JFSCI.2018.08.555736 Journal of Forensic Sciences & Criminal Investigation Chloroform: diethyl ether: methanol: solvent vapor is important.

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