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1.
Barroso M Gallardo E Vieira DN Queiroz JA López-Rivadulla M 《Analytical and bioanalytical chemistry》2011,400(6):1665-1690
The use and abuse of illegal drugs affects all modern societies, and therefore the assessment of drug exposure is an important
task that needs to be accomplished. For this reason, the reliable determination of these drugs and their metabolites in biological
specimens is an issue of utmost relevance for both clinical and forensic toxicology laboratories in their fields of expertise,
including in utero drug exposure, driving under the influence of drugs and drug use in workplace scenarios. Most of the confirmatory
analyses for abused drugs in biological samples are performed by gas chromatographic–mass spectrometric methods, but use of
the more recent and sensitive liquid chromatography–(tandem) mass spectrometry technology is increasing dramatically. This
article reviews recently published articles that describe procedures for the detection of opiates in the most commonly used
human biological matrices, blood and urine, and also in unconventional ones, e.g. oral fluid, hair, and meconium. Special
attention will be paid to sample preparation and chromatographic analysis. 相似文献
2.
Maurer HH 《Analytical and bioanalytical chemistry》2007,388(7):1315-1325
This paper reviews multi-analyte single-stage and tandem liquid chromatography–mass spectrometry (LC-MS) procedures using
different mass analyzers (quadrupole, ion trap, time-of-flight) for screening, identification, and/or quantification of drugs,
poisons, and/or their metabolites in blood, plasma, serum, or urine published after 2004. Basic information about the biosample
assayed, work-up, LC column, mobile phase, ionization type, mass spectral detection mode, and validation data of each procedure
is summarized in tables. The following analytes are covered: drugs of abuse, analgesics, opioids, sedative-hypnotics, benzodiazepines,
antidepressants including selective-serotonin reuptake inhibitors (SSRIs), herbal phenalkylamines (ephedrines), oral antidiabetics,
antiarrhythmics and other cardiovascular drugs, antiretroviral drugs, toxic alkaloids, quaternary ammonium drugs and herbicides,
and dialkylphosphate pesticides. The pros and cons of the reviewed procedures are critically discussed, particularly, the
need for studies on matrix effects, selectivity, analyte stability, and the use of stable-isotope labeled internal standards
instead of unlabeled therapeutic drugs. In conclusion, LC-MS will probably become a gold standard for detection of very low
concentrations particularly in alternative matrices and for quantification in clinical and forensic toxicology. However, some
drawbacks still need to be addressed and finally overcome.
Photos of LC-MS apparatus and typical samples suitable for toxicological analysis 相似文献
3.
Determination of drugs of abuse in blood is of great importance in clinical and forensic toxicology. This review describes
procedures for detection of the following drugs of abuse and their metabolites in whole blood, plasma or serum: Δ9-tetrahydrocannabinol,
11-hydroxy-Δ9-tetrahydrocannabinol, 11-nor-9-carboxy-Δ9-tetrahydrocannabinol, 11-nor-9-carboxy-Δ9-tetrahydrocannabinol glucuronide,
heroin, 6-monoacetylmorphine, morphine, morphine-6-glucuronide, morphine-3-glucuronide, codeine, amphetamine, methamphetamine,
3,4-methylenedioxymethamphetamine, N-ethyl-3,4-methylenedioxyamphetamine, 3,4-methylenedioxyamphetamine, cocaine, benzoylecgonine, ecgonine methyl ester, cocaethylene,
other cocaine metabolites or pyrolysis products (norcocaine, norcocaethylene, norbenzoylecgonine, m-hydroxycocaine, p-hydroxycocaine, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, ethyl ecgonine, ecgonine, anhydroecgonine methyl ester, anhydroecgonine ethyl ester, anhydroecgonine,
noranhydroecgonine, N-hydroxynorcocaine, cocaine N-oxide, anhydroecgonine methyl ester N-oxide). Metabolites and degradation products which are recommended to be monitored for assessment in clinical or forensic
toxicology are mentioned. Papers written in English between 2002 and the beginning of 2007 are reviewed. Analytical methods
are assessed for their suitability in forensic toxicology, where special requirements have to be met. For many of the analytes
sensitive immunological methods for screening are available. Screening and confirmation is mostly done by gas chromatography
(GC)–mass spectrometry (MS) or liquid chromatography (LC)–MS(/MS) procedures. Basic information about the biosample assayed,
internal standard, workup, GC or LC column and mobile phase, detection mode, and validation data for each procedure is summarized
in two tables to facilitate the selection of a method suitable for a specific analytic problem. 相似文献
4.
This review focuses on possible pitfalls in hair testing procedures. Knowledge of such pitfalls is useful when developing
and validating methods, since it can be used to avoid wrong results as well as wrong interpretations of correct results. In
recent years, remarkable advances in sensitive and specific analytical techniques have enabled the analysis of drugs in alternative
biological specimens such as hair. Modern analytical procedures for the determination of drugs in hair specimens—mainly by
gas chromatography–mass spectrometry (GC–MS) and liquid chromatography–mass spectrometry (LC–MS)—are reviewed and critically
discussed. Many tables containing information related to this topic are provided. 相似文献
5.
Peters FT Drvarov O Lottner S Spellmeier A Rieger K Haefeli WE Maurer HH 《Analytical and bioanalytical chemistry》2009,393(2):735-745
Sample preparation for systematic toxicological screening analysis (STA) in urine by gas chromatography–mass spectrometry
(GC-MS) generally involves cleavage of conjugates by acid hydrolysis (Hy) or enzymatic hydrolysis (Gluc) followed by liquid–liquid
extraction (LLE) or solid-phase extraction (SPE), and derivatization, e.g., acetylation (Ac). LLE and derivatization can be
performed simultaneously, e.g., in extractive methylation (ExMe). The work presented consisted of two separate studies. In
study I, 350 urine samples from 168 inpatients from an internal medicine ward were worked up by Hy-LLE-Ac, the standard workup
in the authors’ laboratory, Gluc-SPE-Ac, and Gluc-ExMe. In study II, 100 urine samples from psychiatric inpatients were worked
up by Hy-LLE-Ac and Hy-SPE-Ac. The samples prepared were analyzed by full-scan GC-MS, and the drugs and/or their metabolites/artifacts
detected after the different workup procedures were compared. The results obtained after Hy-LLE-Ac and Gluc-SPE-Ac showed
only little differences, e.g., salicylic acid not being detectable with the latter. Hy-SPE-Ac covered a similar range of analytes
as Hy-LLE-Ac but was much more time-consuming. Comparison of Hy-LLE-Ac and Gluc-ExMe showed that the former was better suited
for basic drugs and the latter for acidic drugs, but the overlap was considerable. In conclusion, Hy-LLE-Ac remains the method
of choice for STA in clinical toxicology owing to its wide analyte spectrum and short workup time. Gluc-ExMe is an ideal complementary
method when acidics need to be covered. Gluc-SPE-Ac can be used as an alternative to Hy-LLE-Ac when turnaround is not critical
or when automated analysis is required.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.
Some of these results were reported at the 46th International TIAFT Meeting, Martinique, 2–8 June 2008. 相似文献
6.
Clinical and forensic toxicology and doping control deal with hundreds or thousands of drugs that may cause poisoning or are
abused, are illicit, or are prohibited in sports. Rapid and reliable screening for all these compounds of different chemical
and pharmaceutical nature, preferably in a single analytical method, is a substantial effort for analytical toxicologists.
Combined chromatography–mass spectrometry techniques with standardised reference libraries have been most commonly used for
the purpose. In the last ten years, the focus has shifted from gas chromatography–mass spectrometry to liquid chromatography–mass
spectrometry, because of progress in instrument technology and partly because of the polarity and low volatility of many new
relevant substances. High-resolution mass spectrometry (HRMS), which enables accurate mass measurement at high resolving power,
has recently evolved to the stage that is rapidly causing a shift from unit-resolution, quadrupole-dominated instrumentation.
The main HRMS techniques today are time-of-flight mass spectrometry and Orbitrap Fourier-transform mass spectrometry. Both
techniques enable a range of different drug-screening strategies that essentially rely on measuring a compound’s or a fragment’s
mass with sufficiently high accuracy that its elemental composition can be determined directly. Accurate mass and isotopic
pattern acts as a filter for confirming the identity of a compound or even identification of an unknown. High mass resolution
is essential for improving confidence in accurate mass results in the analysis of complex biological samples. This review
discusses recent applications of HRMS in analytical toxicology. 相似文献
7.
This paper reviews scientific contributions on the identification and/or quantification of metabolites of drugs of abuse in
in vitro assays or various body samples using hyphenated mass spectrometry. Gas chromatography–mass spectrometry (GC-MS) as
well as liquid chromatography–mass spectrometry (LC-MS) approaches are considered and discussed if they have been reported
in the last five years and are relevant to clinical and forensic toxicology or doping control. Workup and artifact formation
are discussed, and typical examples of studies of the metabolism of designer drugs, doping agents, herbal drugs, and synthetic
cannabinoids are provided. Procedures for quantifying metabolites in body samples for pharmacokinetic studies or in enzyme
incubations for enzyme kinetic studies are also reviewed. In conclusion, the reviewed papers showed that both GC-MS and LC-MS
still have important roles to play in research into the metabolism of drugs of abuse, including doping agents. 相似文献
8.
Maurer HH 《Analytical and bioanalytical chemistry》2005,381(1):110-118
This paper reviews procedures for quantification of drugs in the biosamples blood, plasma, serum, or oral fluid (saliva, etc.) using liquid chromatography coupled with single-stage or tandem mass spectrometry (LC–MS, LC–MS–MS). Such procedures are important prerequisites for competent toxicological judgment and consultation in clinical and forensic toxicology. They cover blood (plasma, serum) analysis of amphetamines and related designer drugs, anesthetics, anticonvulsants, benzodiazepines, opioids, serotonergic drugs, tricyclic antidepressants, neuroleptics, antihistamines, beta-blockers, muscle relaxants, and sulfonylurea-type antidiabetics, and oral fluid analysis of amphetamines and related designer drugs, cocaine, benzoylecgonine, codeine, morphine, enantiomers of methadone and its main metabolite 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), the nicotine metabolites cotinine and hydroxycotinine, and finally risperidone and its metabolite 9-hydroxyrisperidone. Basic information on the procedures is given in two tables and an example of quantification is illustrated in two figures. The pros and cons of such LC–MS procedures including sample work-up and ion suppression effects are critically discussed. 相似文献
9.
The rate of adsorption of water vapor by compounds obtained from cationic copper(II) and nickel(II) ammine complexes and polyoxometallate
anions may be described by the linear driving force mass transfer model as one or two parallel processes. The differences
observed were attributed to differences in the crystal structure of the adsorbents.
__________
Translated from Teoreticheskaya i éksperimental’naya Khimiya, Vol. 43, No. 2, pp. 112–117, March–April, 2007. 相似文献
10.
Current role of LC–MS(/MS) in doping control 总被引:1,自引:0,他引:1
Liquid chromatography–(tandem) mass spectrometry (LC–MS/MS) has revolutionized the detection assays used in doping control
analysis over the last decade. New methods have enabled the determination of drugs that were formerly difficult to detect
or undetectable at preceding sample concentrations, and complex and/or time-consuming procedures based on alternative chromatographic–mass
spectrometric or immunochemical principles have been replaced by faster, more comprehensive and robust assays. A critical
overview of the contributions of LC–MS(/MS) to sports drug testing is provided, including recent developments regarding low
and high molecular weight drugs. 相似文献
11.
Eva Saar Dimitri Gerostamoulos Olaf H. Drummer Jochen Beyer 《Analytical and bioanalytical chemistry》2009,393(2):727-734
Antipsychotic drugs are frequently associated with sudden death investigations. Detection of these drugs is necessary to establish
their use and possible contribution to the death. LC–MS(MS) methods are common; however accurate and precise quantification
is assured by using validated methods. This study compared extraction efficiency and matrix effects using common liquid–liquid
and solid-phase extraction procedures in both ante-mortem and post-mortem specimen using LC–MS–MS. Extraction efficiencies
and matrix effects were determined in five different blank blood specimens of each blood type. The samples were extracted
using a number of different liquid–liquid extraction methods and compared with a standard mixed-mode solid-phase extraction
method. Matrix effects were determined using a post-extraction addition approach—the blank blood specimens were extracted
as described above and the extracts were reconstituted in mobile phase containing a known amount of analytes. The extraction
comparison of ante-mortem and post-mortem blood showed considerable differences, in particular the extraction efficiency was
quite different between ante-mortem and post-mortem blood. Quantitative methods used for determination of antipsychotic drugs
in post-mortem blood should establish that there are no differences in extraction efficiency and matrix effects, particularly
if using ante-mortem blood as calibrator. 相似文献
12.
Erin L. Karschner Allan J. Barnes Ross H. Lowe Karl B. Scheidweiler Marilyn A. Huestis 《Analytical and bioanalytical chemistry》2010,397(2):603-611
A sensitive analytical method for simultaneous quantification of sub-nanogram concentrations of cannabidiol (CBD), Δ9-tetrahydrocannabinol (THC), 11-hydroxy-THC (11-OH-THC), and 11-nor-9-carboxy-THC (THCCOOH) in plasma is presented for monitoring
cannabinoid pharmacotherapy and illicit cannabis use. Analytes were extracted from 1 mL plasma by solid-phase extraction,
derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide with 1% trimethylchlorosilane, and analyzed by two-dimensional gas chromatography
mass spectrometry (2D-GCMS) with cryofocusing. The lower calibration curve was linear from 0.25–25 ng/mL for CBD and THC,
0.125-25 ng/mL for 11-OH-THC and 0.25-50 ng/mL for THCCOOH. A second higher linear range from 5–100 ng/mL, achieved through
modification of injection parameters, was validated for THC, 11-OH-THC, and THCCOOH and was only implemented if concentrations
exceeded the lower curve upper limit of linearity. This procedure prevented laborious re-extraction by allowing the same specimen
to be re-injected for quantification on the high calibration curve. Intra- and inter-assay imprecision, determined at four
quality control concentrations, were ≤7.8% CV. Analytical bias was within ±9.2% of target and extraction efficiencies were
≥72.9% for all analytes. Analytes were stable when stored at 22°C for 16 h, 4°C for 48 h, after three freeze–thaw cycles at
−20°C and when stored on the autosampler for 48 h. This sensitive and specific 2D-GCMS assay provides a new means of simultaneously
quantifying CBD, THC and metabolite biomarkers in clinical medicine, forensic toxicology, workplace drug testing, and driving
under the influence of drugs programs. 相似文献
13.
An overview is given of the existing standards and guidelines for analytical toxicology. Details about guidelines concerning forensic toxicology, clinical toxicology, point-of-care testing, and an area of overlap are provided. Guidelines and standards exist for forensic toxicological analysis in general and for specific situations, e.g., workplace drug testing and driving under the influence of drugs and alcohol. For workplace drug testing, detailed guidelines exist in the U.S.A., Australia, and Europe describing for example the methods used, their cut-off and the process of sample handling. Some governments describe the methods and quality requirements for blood alcohol testing for driving under the influence of alcohol in detail in their laws. In the area of clinical toxicology, guidelines not only focus on the analytical aspects of analysis but also on the timeliness of results. According to the US- and UK-based practice guidelines for the emergency department, the turn-around time should be 1 or 2 h, respectively, for a specific set of analytes. Guidelines are either being developed now or already available (e.g., workplace drug testing, breath alcohol analysis) for point-of-care testing in analytical toxicology. In the context of brain death and sexual assault cases, specific demands need to be imposed because of the unique aspects of drug analysis in these situations (variety of drugs used, low concentrations). Many guidelines and standards are available and it is up to every laboratory to choose the best ones depending on the area of activity and the legal and regulatory environment.Presented at the 10th Conference Quality in the Spotlight, March 2005, Antwerp, Belgium 相似文献
14.
Nola H. Yu Emmie N. M. Ho Terence S. M. Wan April S. Y. Wong 《Analytical and bioanalytical chemistry》2010,396(7):2513-2521
Recombinant human erythropoietin (rhEPO), darbepoetin alfa (DPO) and methoxy polyethylene glycol-epoetin beta (PEG-EPO) are
synthetic analogues of the endogenous hormone erythropoietin (EPO). These erythropoiesis-stimulating agents have the ability
to stimulate the production of red blood cells and are commercially available for the treatment of anaemia in humans. These
drugs are understood to have performance-enhancing effects on human athletes due to their stimulation of red blood cell production,
thereby improving delivery of oxygen to the muscle tissues. Although their effect on horses has not been proven, these substances
were thought to be similarly performance enhancing and have indeed been applied covertly to horses. As such, these protein-based
drugs are prohibited by authorities in both human and equine sports. The method officially adopted by the International Olympic
Committee (IOC) and World Anti Doping Agency (WADA) for the confirmation of rhEPO and/or DPO (rhEPO/DPO) in human urine is
based on electrophoresis in combination with Western blotting. A shortcoming of the WADA method is the lack of definitive
mass spectral data for the confirmation of a positive finding. Recently, a liquid chromatography–tandem mass spectrometry
(LC/MS/MS) method for the detection and confirmation of rhEPO/DPO in equine plasma was reported. However, we have not been
successful in achieving the reported sensitivity. This paper presents a method for the detection and confirmation of rhEPO/DPO,
as well as the newly released PEG-EPO, in equine plasma. The procedures involve immunoaffinity extraction using anti-rhEPO
antibody-coated Dynabeads followed by trypsin digestion. The injected extract was further purified and concentrated using
an on-line trap column in the nano-LC system. Detection and confirmation were achieved by monitoring a unique peptide segment
of rhEPO/DPO/PEG-EPO using nano-liquid chromatography–tandem mass spectrometry equipped with a nanospray ionisation source
operated in the selected reaction monitoring mode. rhEPO, DPO and PEG-EPO can be confirmed at 0.1, 0.2 and 1.0 ng/mL, respectively,
in equine plasma. 相似文献
15.
Liquid chromatography coupled to mass spectrometry nowadays plays an important role in the field of therapeutic drug monitoring
(TDM), especially of new compounds for which no immunoassays are available. This paper reviews LC–MS(–MS) methods published
recently for anti-infective drugs: antiretroviral drugs, other antiviral drugs, antibacterial drugs, antihelmintic drugs,
antimalarial drugs, and other antiprotozoal drugs. An overview of the different methods is given, with special focus on selection
of the internal standard and validation procedures. 相似文献
16.
Maurer HH 《Journal of mass spectrometry : JMS》2006,41(11):1399-1413
Hyphenated mass spectrometric techniques, particularly gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS), are indispensable tools in clinical and forensic toxicology and in doping control owing to their high sensitivity and specificity. They are used for screening, library-assisted identification and quantification of drugs, poisons and their metabolites, prerequisites for competent expertise in these fields. In addition, they allow the study of metabolism of new drugs or poisons as a basis for developing screening procedures in biological matrices, most notably in urine, or toxicological risk assessment. Concepts and procedures using GC/MS and LC/MS techniques in the areas of analytical toxicology and the role of mass spectral libraries are presented and discussed in this feature article. Finally, perspectives of their future position are discussed. 相似文献
17.
Remane D Meyer MR Wissenbach DK Maurer HH 《Analytical and bioanalytical chemistry》2011,400(7):2093-2107
Multi-analyte procedures are of great interest in clinical and forensic toxicology making the analytical process much simpler,
faster, and cheaper and allow monitoring of analytes of different drug classes in one single body sample. The aim of the present
study was to validate an ultra high performance liquid chromatographic-tandem mass spectrometric approach for fast target
screening and quantification of 34 antidepressants in plasma after simple liquid–liquid extraction as part of a multi-analyte
procedure for over 130 drugs. The validation process including recovery, matrix effects, process efficiency, ion suppression/enhancement
of co-eluting analytes (already published), selectivity, cross talk, accuracy and precision, stabilities, and limits of quantification
and detection showed that the approach was selective, sensitive, accurate, and precise for 28 of the 34 tested drugs. The
applicability was successfully tested by analyzing authentic plasma samples and external quality control samples. Furthermore,
it could be shown that time- and cost-saving one-point calibration was applicable for 21 drugs for daily routine and especially
in emergency cases. 相似文献
18.
Nerea Ferreirós Bouzas Sebastian Dresen Barbara Munz Wolfgang Weinmann 《Analytical and bioanalytical chemistry》2009,395(8):2499-2507
A new quantitation method for the determination of drugs of abuse (opiates, amphetamine and derivatives, cocaine, methadone
and metabolites) in serum by using online extraction coupled to liquid chromatography (LC)–mass spectrometry (MS)/MS has been
developed. The online extraction is carried out using two extraction columns simultaneously and one analytical column. One
extraction column is loaded, while the other one is eluted by a gradient. The elution gradient also separates the analytes
in the analytical column. For the sample preparation, serum is spiked with a mixture of deuterated analogues of the drugs.
After protein precipitation with methanol/zinc sulphate, centrifugation, evaporation and reconstitution, the sample is injected
into the LC system. The quantitation is based on the analysis of two multiple reaction monitoring transitions per drug. The
recovery of the protein precipitation step is over 80% for all analytes. Intra- and interday precision, as relative standard
deviation, is lower than 6%, and in the case of accuracy, RE is lower than 15%. Only the most polar analytes showed matrix
effects. The limits of quantitation for the analysed compounds vary between 0.5 and 2.8 ng/mL. The developed method was used
to quantify basic drugs in samples “from driving under the influence of drugs” cases. The results were compared with those
obtained by using solid-phase extraction–GC–MS. 相似文献
19.
Liquid chromatography–(tandem) mass spectrometry [(LC-MS(/MS)] has become an integral part of modern sports drug testing as
it offers unique capabilities complementing immunological and gas chromatography–(tandem) mass spectrometry [(GC-MS(/MS)]-based
detection methods for prohibited compounds. The improved options of fast and sensitive targeted analysis as well as untargeted
screening procedures utilizing high resolution/high accuracy mass spectrometry have considerably expanded the tools available
to anti-doping laboratories for initial testing and confirmation methods. One approach is to focus on pre-selected target
analytes that are measured with utmost specificity and sensitivity using diagnostic precursor–product ion pairs in low resolution
tandem mass spectrometers. The other scenario is to measure and plot extracted ion chromatograms of protonated or deprotonated
molecules as well as product ions as recorded in the full scan mode with high resolution/high accuracy mass spectrometry.
Examples of recent applications of sports drug testing procedures published between 2007 and 2010 are presented and discussed,
outlining the particular advantages of the selected approaches as well as their limitations in a short- and long-term perspective. 相似文献
20.
The role of alternative specimens in toxicological analysis 总被引:1,自引:0,他引:1
The use of alternative specimens in the field of toxicology was first described in 1979, when hair analysis was used to document chronic drug exposure. Since then, the use of these 'alternative' samples has gained tremendous importance in forensic toxicology, as well as in clinic toxicology, doping control and workplace drug testing. It is not surprising, therefore, that a large number of papers dealing with the determination of several classes of drugs in saliva, sweat, meconium and hair have been published ever since, owing to the fact that chromatographic equipment is becoming more and more sensitive, mass spectrometry (and tandem mass spectrometry) being the most widely used analytical tool, combined with gas or liquid chromatography. 'Alternative' specimens present a number of advantages over the 'traditional' samples normally used in toxicology (e.g. blood, urine and tissues), namely the fact that their collection is not invasive, their adulteration is difficult, and they may allow increased windows of detection for certain drugs. The main disadvantage of this kind of samples is that drugs are present in very low concentrations, and therefore high-sensitivity techniques are required to accomplish the analysis. This paper reviews a series of publications on the use of alternative specimens, with special focus on the main analytical and chromatographic problems that these samples present, as well on their advantages and disadvantages over traditional samples in documenting drug exposure. 相似文献