scholarly journals Detection of 6-monoacetylemorphine in hair sample of heroin addicts using gas chromatography–mass spectrometry and significance of rehabilitation program

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Mohsin Ahmad Ghauri ◽  
Fahad Hassan ◽  
Younusa Hassan ◽  
Naveel Atif ◽  
Ahmad Adnan

Abstract Background The analysis of hair samples for the detection of drugs has become one of the convincing strategies in the field of forensic toxicology. A large number of cases concerning heroin abuse or its byproducts have been documented under the Control of Narcotic Substances Act, 1997, over the past decade. The present study was carried out with an aim to evaluate the primary metabolite of heroin, i.e., 6-monoacetylemorphine (6-MAM), in hair samples of addicts and subjects undergoing rehabilitation, thereafter accessing the success rate of the rehabilitation program at the de-addiction center. Results Hair samples were randomly collected from 20 regular heroin addicts and 20 heroin addicts from their past, from the rehabilitation center, of different age groups. Samples were cleaned, digested, and extracted using an alkaline digestion mediator methyl tertiary butyl ether, followed by quantification of 6-MAM via gas chromatography–mass spectrometry (GC–MS). The mean concentration of 6-MAM in regular heroin addicts detected was 7.80 ng/mg and 2.34 ng/mg in samples of subjects undergoing rehabilitation at the de-addiction center, respectively. Conclusion Traces of 6-MAM in the hair sample of heroin addicts can be efficiently detected days after the last intake of heroin. In addition to that, our findings also give an idea for future evaluating the approximate timeframe for detection of 6-MAM and/or other metabolites of heroin in the hair sample. However, in the future, by carefully analyzing the hair samples that can be taken from rehabilitation centers from target subjects at different time intervals, the exact duration of traceable quantity of 6-MAM can be determined in the hair sample. Finally, it can be concluded that there is a significant success rate of the rehabilitation program at de-addiction centers in connection with dragging the 6-MAM level from the body.

Molecules ◽  
2019 ◽  
Vol 24 (13) ◽  
pp. 2501 ◽  
Author(s):  
Nam Hee Kwon ◽  
Yu Rim Lee ◽  
Hee Seung Kim ◽  
Jae Chul Cheong ◽  
Jin Young Kim

Sample preparation is an important step in the isolation of target compounds from complex matrices to perform their reliable and accurate analysis. Hair samples are commonly pulverized or processed as fine cut, depending on preference, before extraction by techniques such as solid-phase extraction (SPE), liquid–liquid extraction, and other methods. In this study, a method based on hybrid solid-phase extraction (hybridSPE) and gas chromatography–mass spectrometry (GC–MS) was developed and validated for the determination of methamphetamine (MA) and amphetamine (AP) in hair. The hair samples were mechanically pulverized after washing with de-ionized water and acetone. The samples were then sonicated in methanol at 50 °C for 1 h and centrifuged at 50,000× g for 3 min. The supernatants were transferred onto the hybridSPE cartridge and extracted using 1 mL of 0.05 M methanolic hydrogen chloride. The combined solutions were evaporated to dryness, derivatized using pentafluoropropionic anhydride, and analyzed by GC–MS. Excellent linearity (R2 > 0.9998) was achieved in the ranges of 0.05–5.0 ng/mg for AP and 0.1–10.0 ng/mg for MA. The recovery was 83.4–96.8%. The intra- and inter-day accuracies were −9.4% to 5.5% and −5.1% to 3.1%, while the intra- and inter-day precisions were within 8.3% and 6.7%, respectively. The limits of detections were 0.016 ng/mg for AP and 0.031 ng/mg for MA. The validated hybridSPE method was applied to dyed hair for MA and AP extraction and compared to a methanol extraction method currently being used in our laboratory. The results showed that an additional hybridSPE step improved the recovery by 5.7% for low-concentration quality control (QC) samples and by 24.1% for high-concentration QC samples. Additionally, the hybridSPE method was compared to polymeric reversed-phase SPE methods, and the absolute recoveries for hybridSPE were 50% and 20% greater for AP (1.5 ng/mg) and MA (3.0 ng/mg), respectively. In short, the hybridSPE technique was shown to minimize the matrix effects, improving GC–MS analysis of hair. Based on the results, the proposed method proved to be effective for the selective determination of MA and AP in hair samples.


Author(s):  
N. A. Al-Abkal ◽  
E. Kh. Metwally ◽  
S. R. Alezzbawy ◽  
Kh. Y. Orabi ◽  
Sh. H. Alshammari

Aim: To compare the main and additive components of heroin trafficked in the Stateof Kuwait during 2012 with those components of heroin traded recently in the country during 2016 and 2017, and to provide a satisfactory explanation for the increase in deaths among heroin addicts during the period2011 -2018. Study Design: Selected samples of non-pure powder heroin seized in Kuwait during 2016 and 2017, with pure heroin and a set of10 pure different heroin component standards, all have been quantitatively analyzed in the Forensic Laboratories. Place and Duration of Study: All qualitative and quantitative analyses for 2016 and 2017 samples were conducted in the Forensic Laboratories of the General Department of Criminal Evidences – Ministry of Interior – State of Kuwait. Methodology: By using Gas Chromatography/Mass Spectrometry (GC/MS) to qualitative and quantitative analysis have been made on a total of hundred samples of non-pure powder heroin seized in Kuwait during the years 2016 and 2017, in addition to ten pure standards. Results: The concentration of the diacetylmorphine (active substance of heroin) in Kuwait during the year 2017 are much higher than the concentration during the year 2016. The additive substances (adulterants) for the years 2016 and 2017, are shared with the year 2012 by the component's paracetamol, caffeine and diazepam with different concentrations. But new adulterants in recent years are recorded in samples 2016 and 2017, including methamphetamine, dextromethorphan, and methylphenidate which is absent in 2016 samples. Conclusion: The concentration % of illicit heroin traded in Kuwait as diacetylmorphine has increase from 10% to 50% for year 2016, and further from 30% - 70% for year 2017, which marks identified a substantial rising in the purity of heroin. In addition, additive substances in the two years include paracetamol (acetaminophen), caffeine and diazepam, previously recorded in 2012. However, totally different new adulterates are recorded in 2016 and 2017 samples, including methamphetamine, dextromethorphan, and methylphenidate. All new three adulterates are detected in quite a few numbers of samples with methylphenidate recorded in a very low concentration of 0. 01 mg. Both new adulterates and higher purity of heroin constitute the main reasons for rising the rate of deaths between heroin addicts in recent years. Also, recent UN reports (12,18) provide evidence that the GC countries Afghanistan, Iran and Pakistan are still manufacturing and trading the above mentioned new adulterates.


Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5739
Author(s):  
Keita Saito ◽  
Yoshiyuki Tokorodani ◽  
Chihiro Sakamoto ◽  
Hiroyuki Kataoka

The odors and emanations released from the human body can provide important information about the health status of individuals and the presence or absence of diseases. Since these components often emanate from the body surface in very small quantities, a simple sampling and sensitive analytical method is required. In this study, we developed a non-invasive analytical method for the measurement of the body odor component 2-nonenal by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry by selective ion monitoring. Using a StableFlex PDMS/DVB fiber, 2-nonenal was efficiently extracted and enriched by fiber exposition at 50℃ for 45 min and was separated within 10 min using a DB−1 capillary column. Body odor sample was easily collected by gauze wiping. The limit of detection of 2-nonenal collected in gauze was 22 pg (S/N=3), and the linearity was obtained in the range of 1−50 ng with a correlation coefficient of 0.991. The method successfully analyzed 2-nonenal in skin emissions and secretions and was applied to the analysis of body odor changes in various lifestyles, including the use of cosmetics, food intake, cigarette smoking, and stress load.


Author(s):  
Pham Quoc Chinh ◽  
Pham Thi Thu Ha ◽  
Nguyen Mai Dung ◽  
Vu Huu Phuoc ◽  
Vu Duc Loi ◽  
...  

This article develops a combined solid phase extraction (SPE) and gas chromatography – mass spectrometry (GC-MS) procedure for determining amphetamine-type stimulants Amphetamine (AM) and Methamphetamine (MA) in human hair. Hair samples were incubated in methanol containing 1% hydrochloric acid in 18 hours and then subjected to SPE. The obtained extracts were evaporated to dryness, derivatized with heptafluorobutyric anhydride (HFBA) at 70 °C for 30 minutes prior to GC–MS analysis. Gas chromatography mass spectrometry was run on HP5-MS column (30 m × 0.25 mm × 0.25 µm) with detector MS 5975C. Experimentally, the proposed method proved sensitive, simple and time-saving, but quite accurate with a low limit of detection (LOD = 0.05ng/mg) and quantitation (LOQ = 0.15ng/mg). Keywords: SPE, GC – MS, hair samples, amphetamine, methamphetamine. References [1] Ming-Ren Fuh, Ti-Yu Wu and Tzuen-Yeuan Lin, Determination of amphetamine and methamphetamine in urine by solid phase extraction and ion-pair liquid chromatography–electrospray–tandem mass spectrometry Talanta, 68 (3) (2006), 987-991. https://doi.org/10.1016/j.talanta.2005.06.057[2] Naresh C. Jain, Thomas C. Sneath, and Robert D. Budd, Rapid Gas-Chomatographic Determination of Amphetamine and Methamphetamine in urine, Clinical Chemistry, 20 (11) (1974) 1460-1462. https://doi.org/10.1093/clinchem/20.11.1460.[3] Dong-liang Lin, Rea-Ming Yin, Ray H. Liu, Gas Chromatography-Mass Spectrometry (GC-MS) Analysis of Amphetamine, Methamphetamine, 3,4-Methylenedioxy- amphetamine and 3,4-Methylenedioxymethamphetamine in Human Hair and Hair Sections, Journal of Food and Drug Analysis, 13(2) (2005) 193-200. https://doi.org/10.38212/2224-6614.2526[4] María Jesús Tabernero, Maria Linda Felli, Ana María Bermejo, Marcello Chiarotti, Determination of ketamine and amphetamines in hair by LC/MS/MS, Anal Bioanal Chem, 395(2009), 2547–2557. https://doi.org/10.1007/s00216-009-3163-4.[5] D.V. Doan, D.Q. Huy, N.D. Hue, T.M. Tri, Determination of methamphetamine in urine samples by gas chromatography mass spectrometry combined with solid phase extraction technique, Journal of Science and Technology 47 (6) (2009) 53-58 (in Vietnamese).[6] Rodger L. Foltz, Allison F. Fentiman, Ruth B. Foltz, GC/MS Assays for Abused Drugs in Body Fluids, National Institute on Drug Abuse, Maryland, 1980.[7] AOAC, Appendix F: Guidelines for Standard Method Performance Requirements, AOAC official methods of analysis, Maryland, 2016.[8] Eunyoung Han, Martin P. Paulus, Marc Wittmann, Heesun Chung, Joon myong Song, Hair analysis and self-report of methamphetamine use by methamphetamine dependent individuals, Journal of Chromatography B, 879 (2011) 541–547. https://doi.org/10.1016/j.jchromb.2011.01.002.      


1999 ◽  
Vol 45 (9) ◽  
pp. 1485-1494 ◽  
Author(s):  
Robert Kronstrand ◽  
Sophie Förstberg-Peterson ◽  
Bertil KÅgedal ◽  
Johan Ahlner ◽  
Göran Larson

Abstract Background: Analysis of drugs in hair has been used on a qualitative basis to estimate earlier exposure to drugs. Clinical applications are rare because of the lack of dose–response relationships in the studies performed to date, and questions remain regarding the mechanisms of drug incorporation into hair. Several human studies have shown differences in drug accumulation between pigmented and nonpigmented hair. However, the melanin concentration in hair was not determined and correlated to the amount of drug incorporated. Methods: Nine human subjects were given codeine as a single oral dose, and plasma codeine concentrations were determined for 24 h, using gas chromatography–mass spectrometry. Hair samples were obtained weekly for a month. Total melanin, eumelanin, and codeine were measured quantitatively in hair samples by spectrophotometry, HPLC, and gas chromatography–mass spectrometry, respectively. Results: There was an exponential relationship between codeine and melanin concentrations in hair, (r2 = 0.95 with total melanin and r2 = 0.83 with eumelanin). After normalizing the results by the area under the curve for codeine in plasma, we obtained r2 = 0.86 for codeine vs total melanin and r2 = 0.90 vs eumelanin. Conclusions: Our results stress the importance of melanin determination when measuring drugs in hair. We postulate that analysis of drug concentration in hair may be worthwhile in the monitoring of drug compliance if the results are normalized for melanin content.


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