April - June 2010 - Bureau of Police Research and Development

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Detection of Lorazepam from Human Viscera by a new HPLC technique(b) 1% DPA in acetone followed by exposure to UVfor Organochloro and(c) Tollens reagent and heat at 1100C for 05 minutesfor Carbamates.Along withconventionaltechniques/methodsadopted forexamination of thecase, a nonconventionalmobilephase was used inHPLC, which has beensuccessfully applied.FTIR spectra No-1(FTIR spectra of standard Lorazepam)FTIR spectra No-2[Overlay spectra of standard Lorazepam(black) andextract of trapex tablets (red).]exhibits to contain lorazepam as the activeingredient (FTIR spectra no- 2). The main objectiveof the examination was now focused on theexamination of the viscera to know whether anydrugs/poison was present in them. Some part ofthe stomach with its contents, small intestine with itcontents and liver gall bladder, etc. was extractedwith n-Hexane. The TLC was done with the n-hexaneextract along with a known standard to detect thepresence of common poisons like Organochloro,Organophosphorous and Carbamates group ofpesticides, if any.TLC System: Hexane : Acetone :: 9: 1,Visualisation under UV 254 nmSpray reagents(a) Palladium chloride for Organophosphorous,Observation of TLC Studies: No spot or streak norany colour development corresponding to thestandard pesticide. Thus, the presence of pesticidethat might be the plausible cause of death in thiscase is ruled out.The other parts of the viscera samples weresubjected to stepwise extraction for the presenceof drugs. The samples were added acetic acid andsaturated Ammonium Sulphate and heated at 60-70oc in a water for about six hrs and filtered afterfollowing other standard procedures. The filtrateextracted with Di-ethyl ether, which is the acidicextract, liquid part, made basic by adding ammoniaand extracted with chloroform, which is the basicextract. The concentrated extract was taken andinitially done TLC for screening the class of drugsthat might be present in them.TLC system: (I) Chloroform: Acetone :: 4:1(II) Chloroform: methanol:: 9 :1Visualisation under UV 254 nmSpray reagent- Acidified Potassium Iodo-Platinate for acid extractDraggendorf's reagent forbasic extract.The acidic extract of the viscera revealed thepresence of a benzodiazepine the Rf value wasalmost similar to that of lorazepam.Instrumental studies II- The samples were scrappedout after a preparative TLC and filtered by MilliporeMilex -HV Nylon 0.45um filter discs to remove thepresence of foreign particles, if any. Initially, it wasproposed to analyse the samples with GC-MS butliterature studies reveal that lorazepam is notthermally stable and a number of investigations haveshown that under gas chromatographic conditions42 ➢ The Indian Police Journal Vol. LVII-No. 2, April-June, 2010
Detection of Lorazepam from Human Viscera by a new HPLC techniquelorazepam can loose a water molecule and rearrangeto form 6-chloro-4-(2'-chlorophenyl quinazoline)-2-carboxaldehyde. Consequently, in a gaschromatographic procedure where lorazepam isinjected directly this rearrangement must beconsidered. Another consideration is that in metabolicstudies the major metabolite is excreted as theglucorunide and preliminary enzymatic incubationis employed. However such problems can beremoved by conversion of lorazepam to itsbenzophenone derivative prior to injection.In this case the problem of metabolite disintegrationwas not important as the TLC studies gaveindications of the presence of the benzodiazepineand the identification of the said particular drug couldprovide a vital clue to the investigating agencies.The case history and Post Mortem report indicatesthat the deceased died within a short while afterconsumption of the drug, probably due to its overdoseand the stomach contents found with some whitegranular sediment were sent for examination. Andin spite of all precautions some amount of fatmaterials mixed with scrapings may give rise toconfusing results as well as may cause damage tothe capillary column.The best suitable alternative was to identify the drugby the High Performance Liquid Chromatography(HPLC) technique. As there was no involvement ofelevated temperature in this technique, thepossibility of the disintegration of the drug can beruled out. From the studies it was revealed that themobile phase for a reverse phase technique of theHPLC was Methanol: Water: Phosphate Buffer(0.1M)at two different v/v/v concentrations and pH 7.25/7.67 (DFS Working Manual, 2005). But due to nonavailability of the buffer and its delay in procurement,during the search for alternative mobile phase it wasfound that benzodiazepines like lorazepam could beanalyzed by HPLC and separated from its degradationproducts by eluent consisting of acidic aqueousacetonitrile on a reverse phase column. The sampleswere analyzed by HPLC with the following analyticalparameters :HPLC methodologyMobile phase : Acetonitrile: Water (70:30) madeslightly acidic,Column - C 18, 5μm, 4.6x150mm, Waters,Pump mode - Isocratic, Flow rate - 1 ml/min,Wave length - 240 nm, Detector - Waters 2487 DualAbsorbance DetectorPump - Waters 1525 Binary HPLC pumpData mode - Absorbance A (Channel-1)Run time - 12 minutesInitially, the standard Lorazepam was injected andinjections were made with different conc. to confirmthe presence of the compound and check therepeatability of the retention time. The retention timewas observed to be 2.353 minutes (HPLCchromatogram no-1). Following was injected theunknown samples, first the extract of the remainingHPLC chromatogram No.-1(HPLC chromatogram of standard Lorazepam)tablet, remaining traces of white powder and lastlythe viscera extract. Repeated injections were madewith varying conc. except for the viscera extract.The Indian Police Journal Vol. LVII-No. 2, April-June, 2010 43➢
Page 1: Vol. LVII-No.2APRIL-JUNE, 2010Edito
Page 4 and 5: Abstracts & Key WordsPolice Sub-Cul
Page 9 and 10: Police Sub-Culture : An Adaptation
Page 11 and 12: Police Sub-Culture : An Adaptation
Page 13 and 14: IntroductionSingapore Community Pol
Page 15 and 16: Singapore Community Policing Experi
Page 17 and 18: Singapore Community Policing Experi
Page 19 and 20: Relevance of KPAs & KPIs in Policin
Page 25 and 26: Conviction Rate : A Reality CheckSh
Page 27 and 28: Conviction Rate : A Reality Checkor
Page 29 and 30: Conviction Rate : A Reality Checkof
Page 31 and 32: Conviction Rate : A Reality Checkco
Page 33 and 34: Conviction Rate : A Reality Checkpe
Page 35 and 36: Conviction Rate : A Reality CheckCo
Page 37 and 38: Cell Tower Radiation Hazard: Need f
Page 39 and 40: Cell Tower Radiation Hazard: Need f
Page 41: Detection of Lorazepam from Human V
Page 45 and 46: Detection of Lorazepam from Human V
Page 47 and 48: Domestic Violence against Women and
Page 49 and 50: Domestic Violence against Women and
Page 51 and 52: IntroductionA Study of Burnout and
Page 53 and 54: A Study of Burnout and Marital Adju
Page 59 and 60: anger has emanated against Pakistan
Page 61 and 62: e overcome and citizens forums and
Page 63 and 64: Marital Rape : The Assasination of
Page 73 and 74: Silence of the Law on Marital RapeG
Page 75 and 76: Silence of the Law on Marital Rapea
Page 77 and 78: Silence of the Law on Marital Rapeo
Page 79 and 80: Silence of the Law on Marital Rapeb
Page 81 and 82: CorrigendumIn Jan-March, 2010 issue
Page 83: James M Klatell (Aug 2006) : Bomb T

April - June 2010 - Bureau of Police Research and Development

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