期刊论文详细信息
Chemistry Central Journal
Hair-based rapid analyses for multiple drugs in forensics and doping: application of dynamic multiple reaction monitoring with LC-MS/MS
Declan P Naughton3  Márta Ránky2  Martina Uvacsek1  Andrea Petroczi3  Iltaf Shah3 
[1]Faculty of Physical Education and Sports Sciences, Semmelweis University, Budapest, Hungary
[2]Eötvös Lóránd University, Faculty of Education and Psychology, Budapest, Hungary
[3]School of Life Sciences, Kingston University, Kingston-upon-Thames, Surrey, UK
关键词: Drugs of abuse;    Toxicology;    Forensics;    Doping;    Controlled drugs;    Human hair;    LC-MS/MS;    Dynamic MRM;   
Others  :  1082299
DOI  :  10.1186/s13065-014-0073-0
 received in 2014-09-19, accepted in 2014-11-26,  发布年份 2014
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【 摘 要 】

Background

Considerable efforts are being extended to develop more effective methods to detect drugs in forensic science for applications such as preventing doping in sport. The aim of this study was to develop a sensitive and accurate method for analytes of forensic and toxicological nature in human hair at sub-pg levels.

Results

The hair test covers a range of different classes of drugs and metabolites of forensic and toxicological nature including selected anabolic steroids, cocaine, amphetamines, cannabinoids, opiates, bronchodilators, phencyclidine and ketamine. For extraction purposes, the hair samples were decontaminated using dichloromethane, ground and treated with 1 M sodium hydroxide and neutralised with hydrochloric acid and phosphate buffer and the homogenate was later extracted with hexane using liquid-liquid extraction (LLE). Following extraction from hair samples, drug-screening employed liquid chromatography coupled to tandem mass spectrometric (LC-MS/MS) analysis using dynamic multiple reaction monitoring (DYN-MRM) method using proprietary software. The screening method (for > 200 drugs/metabolites) was calibrated with a tailored drug mixture and was validated for 20 selected drugs for this study. Using standard additions to hair sample extracts, validation was in line with FDA guidance. A Zorbax Eclipse plus C18 (2.1 mm internal diameter × 100 mm length × 1.8 μm particle size) column was used for analysis. Total instrument run time was 8 minutes with no noted matrix interferences. The LOD of compounds ranged between 0.05-0.5 pg/mg of hair. 233 human hair samples were screened using this new method and samples were confirmed positive for 20 different drugs, mainly steroids and drugs of abuse.

Conclusions

This is the first report of the application of this proprietary system to investigate the presence of drugs in human hair samples. The method is selective, sensitive and robust for the screening and confirmation of multiple drugs in a single analysis and has potential as a very useful tool for the analysis of large array of controlled substances and drugs of abuse.

【 授权许可】

   
2014 Shah et al.; licensee Springer.

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【 参考文献 】
  • [1]Verstraete AG: Detection times of drugs of abuse in blood, urine, and oral fluid. Ther Drug Monit 2004, 26:200-205.
  • [2]Kintz P, Cirimele V, Sachs H, Jeanneau T, Ludes B: Testing for anabolic steroids in hair from two bodybuilders. Forensic Sci Int 1999, 101:209-216.
  • [3]Kronstrand R, Nyström I, Strandberg J, Druid H: Screening for drugs of abuse in hair with ion spray LC–MS–MS. Forensic Sci Int 2004, 145:183-190.
  • [4]Strahm E, Sottas P-E, Schweizer C, Saugy M, Dvorak J, Saudan C: Steroid profiles of professional soccer players: an international comparative study. B J Sports Med 2009, 43:1126-1130.
  • [5]Kintz P: Testing for anabolic steroids in hair: a review. Legal Med 2003, 5:S29-S33.
  • [6]Deshmukh N, Hussain I, Barker J, Petroczi A, Naughton DP: Analysis of anabolic steroids in human hair using LC–MS/MS. Steroids 2010, 75:710-714.
  • [7]Shen M, Xiang P, Shen B, Bu J, Wang M: Physiological concentrations of anabolic steroids in human hair. Forensic Sci Int 2009, 184:32-36.
  • [8]Gosetti F, Mazzucco E, Gennaro MC, Marengo E: Ultra high performance liquid chromatography tandem mass spectrometry determination and profiling of prohibited steroids in human biological matrices. A review J Chromatog B 2013, 927:22-36.
  • [9]Gambelunghe C, Sommavilla M, Ferranti C, Rossi R, Aroni K, Manes N, Bacci M: Analysis of anabolic steroids in hair by GC/MS/MS. Biomed Chromatogr 2007, 21:369-375.
  • [10]Strano-Rossi S, Castrignanò E, Anzillotti L, Odoardi S, De-Giorgio F, Bermejo A, Pascali VL: Screening for exogenous androgen anabolic steroids in human hair by liquid chromatography/orbitrap-high resolution mass spectrometry. Anal Chim Acta 2013, 793:61-71.
  • [11]Vincenti M, Salomone A, Gerace E, Pirro V: Application of mass spectrometry to hair analysis for forensic toxicological investigations. Mass Spectrom Rev 2013, 32:312-332.
  • [12]Gomez C, Fabregat A, Pozo ÓJ, Marcos J, Segura J, Ventura R: Analytical strategies based on mass spectrometric techniques for the study of steroid metabolism. TRAC 2014, 53:106-116.
  • [13]Pötsch L, Skopp G, Moeller MR: Biochemical approach on the conservation of drug molecules during hair fiber formation. Forensic Sci Int 1997, 84:25-35.
  • [14]Pragst F, Balikova MA: State of the art in hair analysis for detection of drug and alcohol abuse. Clin Chim Acta 2006, 370:17-49.
  • [15]Nielen MW, Lasaroms JJ, Mulder PP, Van Hende J, van Rhijn JHA, Groot MJ: Multi residue screening of intact testosterone esters and boldenone undecylenate in bovine hair using liquid chromatography electrospray tandem mass spectrometry. J Chromatogr B 2006, 830:126-134.
  • [16]Gaillard Y, Pépin G: Testing hair for pharmaceuticals. J Chromatogr B 1999, 733:231-246.
  • [17]Rusevska K, Zdravkovski Z: Simple extraction method for detecting exogenous substances in scalp hair by GC-MS. J Hyg Eng Des 2013, 2:59-67.
  • [18]Calvo D, Tort N, Salvador JP, Marco M-P, Centi F, Marco S: Preliminary study for simultaneous detection and quantification of androgenic anabolic steroids using ELISA and pattern recognition techniques. Analyst 2011, 136:4045-4052.
  • [19]Thieme D, Anielski P, Grosse J, Sachs H, Mueller R: Identifcation of anabolic steroids in serum, urine, sweat and hair: comparison of metabolic patterns. Anal Chim Acta 2003, 483:299-306.
  • [20]Herrin GL, McCurdy HH, Wall WH: Investigation of an LC-MS-MS (QTrap®) method for the rapid screening and identification of drugs in postmortem toxicology whole blood samples. J Anal Toxicol 2005, 29:599-606.
  • [21]Viette V, Guillarme D, Mylonas R, Mauron Y, Fathi M, Rudaz S, Hochstrasser D, Veuthey JL: A multi-target screening analysis in human plasma using fast liquid chromatography–hybrid tandem mass spectrometry (Part I). Clin Biochem 2011, 44:32-44.
  • [22]Leung GN, Leung DK, Wan TS, Wong CH: High throughput screening of sub-ppb levels of basic drugs in equine plasma by liquid chromatography–tandem mass spectrometry. J Chromatogr A 2007, 1156:271-279.
  • [23]Vincenti M, Cavanna D, Gerace E, Pirro V, Petrarulo M, Di Corcia D, Salomone A: Fast screening of 88 pharmaceutical drugs and metabolites in whole blood by ultrahigh-performance liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 2013, 405:863-879.
  • [24]Maurer HH: What is the future of (ultra) high performance liquid chromatography coupled to low and high resolution mass spectrometry for toxicological drug screening? J Chromatogr A 2013, 1292:19-24.
  • [25]Montesano C, Johansen SS, Nielsen MKK: Validation of a method for the targeted analysis of 96 drugs in hair by UPLC–MS/MS. J Pharm Biomed Anal 2014, 88:295-306.
  • [26]Oberacher H, Schubert B, Libiseller K, Schweissgut A: Detection and identification of drugs and toxicants in human body fluids by liquid chromatography–tandem mass spectrometry under data-dependent acquisition control and automated database search. Anal Chim Acta 2013, 770:121-131.
  • [27]Dresen S, Ferreiros N, Gnann H, Zimmermann R, Weinmann W: Detection and identification of 700 drugs by multi-target screening with a 3200 Q TRAP® LC-MS/MS system and library searching. Anal Bioanal Chem 2010, 396:2425-2434.
  • [28]Mueller C, Weinmann W, Dresen S, Schreiber A, Gergov M: Development of a multi-target screening analysis for 301 drugs using a QTrap liquid chromatography/tandem mass spectrometry system and automated library searching. Rapid Commun Mass Spectrom 2005, 19:1332-1338.
  • [29]Niessen W: Fragmentation of toxicologically relevant drugs in negative ion liquid chromatography–tandem mass spectrometry. Mass Spectrom Rev 2012, 31:626-665.
  • [30]Broecker S, Herre S, Wüst B, Zweigenbaum J, Pragst F: Development and practical application of a library of CID accurate mass spectra of more than 2,500 toxic compounds for systematic toxicological analysis by LC–QTOF-MS with data-dependent acquisition. Anal Bioanal Chem 2011, 400:101-117.
  • [31]Broecker S, Herre S, Pragst F: General unknown screening in hair by liquid chromatography–hybrid quadrupole time-of-flight mass spectrometry (LC–QTOF-MS). Forensic Sci Int 2012, 218:68-81.
  • [32]Polettini A, Gottardo R, Pascali JP, Tagliaro F: Implementation and performance evaluation of a database of chemical formulas for the screening of pharmaco/toxicologically relevant compounds in biological samples using electrospray ionization-time-of-flight mass spectrometry. Anal Chem 2008, 80:3050-3057.
  • [33]Jamin EL, Bonvallot N, Tremblay-Franco M, Cravedi J-P, Chevrier C, Cordier S, Debrauwer L: Untargeted profiling of pesticide metabolites by LC–HRMS: an exposomics tool for human exposure evaluation. Anal Bioanal Chem 2014, 406:1149-1161.
  • [34]Nielsen MKK, Johansen SS, Dalsgaard PW, Linnet K: Simultaneous screening and quantification of 52 common pharmaceuticals and drugs of abuse in hair using UPLC–TOF-MS. Forensic Sci Int 2010, 196:85-92.
  • [35]Agilent Technical Overview (2007). Ion optics innovations for increased sensitivity in hybrid MS systems. Agilent Technologies USA 5989-7408EN. (http://www.chem.agilent.com/Library/technicaloverviews/Public/5989-7408EN_HI.pdf).
  • [36]Peter S, Thomas G, Frank K, Tim S, M K (2009). New dynamic MRM mode improves data quality and triple quad quantification in complex analyses. Agilent Technologies USA 5990-3595EN. (http://www.chem.agilent.com/Library/technicaloverviews/Public/5990-3595en_lo%20CMS.pdf).
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