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1.
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
2.
Fanny Kieken Gaud Pinel Jean-Philippe Antignac Fabrice Monteau Anne Christelle Paris Marie-Agnès Popot Yves Bonnaire Bruno Le Bizec 《Analytical and bioanalytical chemistry》2009,394(8):2119-2128
Despite the worldwide existing regulation banning the use of the recombinant equine growth hormone (reGH) as growth promoter,
it is suspected to be used in horseracing to improve performances. Various analytical methods previously developed to screen
for its misuse have encountered some limitations in terms of detection timeframes, in particular during the first days following
reGH administration. A novel strategy involving the characterization of global metabolomic fingerprints in urine samples of
non-treated and reGH-treated horses by liquid chromatography–electrospray–high-resolution mass spectrometry (LC-ESI-HRMS)
is described and assessed in this paper in order to develop a new screening tool for growth hormone abuse in horseracing.
The strategy involves a limited sample preparation of the urine samples and the use of appropriate software for data processing
and analysis. As preliminary work, reproducibility of both sample preparation and mass spectrometry (MS) measurements was
evaluated in order to demonstrate the reliability of the method. Application of the developed protocol on two horses demonstrated
the suitability of the developed strategy and preliminary results showed significant modifications of the metabolome after
treatment with reGH.
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3.
Glutathione peroxidase (isolated from bovine erythrocytes) and its behaviour during alkylation and enzymatic digestion were
studied by various hyphenated techniques: gel electrophoresis–laser ablation (LA) inductively coupled plasma (ICP) mass spectrometry
(MS), size-exclusion liquid chromatography–ICP MS, capillary high-performance liquid chromatography (capHPLC)–ICP MS, matrix-assisted
laser desorption/ionization (MALDI) time-of-flight (TOF) MS, electrospray MS, and nanoHPLC–electrospray ionization (ESI) MS/MS.
ESI TOF MS and MALDI TOF MS allowed the determination of the molecular mass but could not confirm the presence of selenium
in the protein. The purity of the protein with respect to selenium species could be evaluated by LA ICP MS and size-exclusion
chromatography (SEC)–ICP MS under denaturating and nondenaturating conditions, respectively. SEC–ICP MS and capHPLC–ICP MS
turned out to be valuable techniques to study the enzymolysis efficiency, miscleavage and artefact formation during derivatization
and tryptic digestion. For the first time the parallel ICP MS and ESI MS/MS data are reported for the selenocysteine-containing
peptide extracted from the gel; capHPLC–ICP MS allowed the sensitive detection of the selenopeptide regardless of the matrix
and nanoHPLC–electrospray made possible its identification.
Figure Eye catching image
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
4.
Stir bar sorptive extraction in combination with thermal desorption coupled online to capillary gas chromatography–mass spectrometry
was applied to investigate volatile and semivolatile fractions in two waste leachate samples: old and fresh ones. The present
study helps to improve our knowledge of waste leachate organic composition. The aim is to then make use of this knowledge
afterwards in order to generate more reliable and specific treatment processes for waste leachates and thus to respect the
environmental statute law regarding their rejection. The volatile and semivolatile compounds appeared to be mainly anthropogenic
in origin. Moreover, lactic acid and cyclic octaatomic sulfur could potentially be used as microbiological activity indicators,
since they occur during organic matter degradation processes within waste leachates.
Figure TDU-CGC-MS analytical equipment 相似文献
5.
Sergi M Bafile E Compagnone D Curini R D'Ascenzo G Romolo FS 《Analytical and bioanalytical chemistry》2009,393(2):709-718
An analytical procedure for the simultaneous determination in human plasma and oral fluids of several illicit drugs belonging
to different chemical and toxicological classes is presented. Amphetamine, methamphetamine, morphine, 6-monoacetylmorphine,
methylenedioxyamphetamine, methylenedioxyethylamphetamine, methylenedioxymethamphetamine, cocaine, benzoylecgonine, tetrahydrocannabinol,
carboxytetrahydrocannabinol, ketamine, and phencyclidine have been quantified in real samples using a very rapid sample treatment,
basically a protein precipitation. The quantitative analysis was performed by liquid chromatography–tandem mass spectrometry
and has been fully validated. All the analytes were detected in positive ionization mode using a TurboIonSpray source, except
carboxytetrahydrocannabinol, which was detected in negative ionization mode. The use of a diverter valve between the column
and the mass spectrometer allows the preservation of the ion source performances for high-throughput analysis.
Figure Diverter system 相似文献
6.
Nattikarn Kaewkhomdee Sandra Mounicou Joanna Szpunar Ryszard Lobinski Juwadee Shiowatana 《Analytical and bioanalytical chemistry》2010,396(3):1355-1364
Sequential extraction (water, Driselase, protease XIV) and extraction with simulated gastric and intestinal fluids were proposed
to characterize the binding and the bioaccessibility of chromium in two commercial food supplements obtained by incorporation
of this element into yeast. Chromium in Cr-enriched yeast was found to be hardly extractable with water, Driselase, or simulated
gastric fluid (recoveries of approximately 10–20%), but proteolysis or gastrointestinal fluid digestion released more than
half of the chromium present. Fractionation with size-exclusion chromatography with Cr-specific detection by inductively coupled
plasma mass spectrometry (ICP MS) allowed the distinction of two fractions: one below approximately 1 kDa and one 1–5 kDa;
they contained the entirety of the released Cr with proportions varying as a function of the extracting solution and the origin
of sample. When collected and investigated by reversed-phase high-performance liquid chromatography–ICP MS, the low molecular
mass fraction was found to release Cr(III), whereas the heavier one showed most of Cr bound in fairly stable hydrophobic complexes.
However, an attempt of their identification by electrospray ionization MS/MS and matrix-assisted laser desorption ionization
MS was not successful.
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7.
Thevis M Geyer H Mareck U Sigmund G Henke J Henke L Schänzer W 《Analytical and bioanalytical chemistry》2007,388(7):1539-1543
Manipulation of urine sampling in sports drug testing is considered a violation of anti-doping rules and is consequently sanctioned
by regulatory authorities. In 2003, three identical urine specimens were provided by three different athletes, and the identity
of all urine samples was detected and substantiated using numerous analytical strategies including gas chromatography–mass
spectrometry with steroid and metabolite profiling, gas chromatography–nitrogen/phosphorus detector analysis, high-performance
liquid chromatography–UV fingerprinting, and DNA-STR (short tandem repeat) analysis. None of the respective athletes was the
donor of the urine provided for doping analysis, which proved to be a urine sample collected from other unidentified individual(s).
Samples were considered suspicious based on identical steroid profiles, one of the most important parameters for specimen
individualization in sports drug testing. A database containing 14,224 urinary steroid profiles of athletes was screened for
specific values of 4 characteristic parameters (ratios of testosterone/epitestosterone, androsterone/etiocholanolone, androsterone/testosterone,
and 5α-androstane-3α,17β-diol/5β-androstane-3α,17β-diol) and only the three suspicious samples matched all criteria. Further
metabolite profiling regarding indicated medications and high-performance liquid chromatography–UV fingerprinting substantiated
the assumption of manipulation. DNA-STR analyses unequivocally confirmed that the 3 urine samples were from the same individual
and not from the athletes who provided DNA from either buccal cell material or blood specimens. This supportive evidence led
to punishment of all three athletes according to the rules of the World Anti-Doping Agency. Application of a new multidisciplinary
strategy employing common and new doping control assays enables the detection of urine substitution in sports drug testing.
Figure Identical GC-MS/NPD profiles of three urine specimens collected from three different individuals for doping control purposes 相似文献
8.
Kallio M Jussila M Raimi P Hyötyläinen T 《Analytical and bioanalytical chemistry》2008,391(6):2357-2363
A previously constructed semi-rotating cryogenic modulator was modified for comprehensive two-dimensional gas chromatography
(GC×GC). The retention time repeatability was improved by replacing the modulator control program unit with a new system.
Peak widths obtained with the modified modulator were comparable with those obtained with the previous modulator and other
modulator types. The modulator was easy to construct and it can be installed in any commercial GC system. The constructed
GC×GC–FID system and data obtained by gas chromatography–mass spectrometry (GC–MS) were used for identification of unknowns
in forest aerosol samples.
Figure A semi-rotating cryogenic modulator in which modulation is based on two-step cryogenic trapping with continuously flowing
carbon dioxide has been developed for comprehensive two-dimensional gas chromatography 相似文献
9.
This paper describes a liquid chromatographic/tandem mass spectrometric (LC/MS–MS) method specifically designed for the screening
of synthetic glucocorticosteroids in human urine. The method is designed to recognize a common mass spectral fragment formed
from the particular portion of the molecular structure that is common to all synthetic glucocorticosteroids and that is fundamental
to their pharmacological activity. As such, the method is also suitable for detecting unknown substances, provided they contain
the portion of the molecular structure selected as the analytical target. The effectiveness of this approach was evaluated
on seventeen synthetic glucocorticosteroids. Urine samples, including blank urines spiked with one or more synthetic glucocorticosteroids,
were treated according to a standard procedure (enzymatic hydrolysis, liquid/liquid extraction and evaporation to dryness)
and analyzed using LC/MS-MS with electrospray ionization (ESI). MS–MS acquisition was carried out in a precursor ion scan,
and the results were compared with those obtained by a previously developed reference technique based on acquisition in the
multiple reaction monitoring (MRM) mode. All of the glucocorticosteroids considered in this study are clearly detectable in
urine, with a limit of detection in the concentration range 5–20 ng/mL, depending on the glucocorticosteroid structure. The
proposed method is therefore suitable for the detection of glucocorticosteroids in urine samples taken for “in competition”
sport anti-doping control tests, matching the requirements of the World Anti-Doping Agency (WADA) for accredited anti-doping
laboratories.
Figure Structures of the synthetic glucocorticoids considered in this study 相似文献
10.
Martínez Ocaña R Mena Granero A Egea Gonzalez FJ Garrido Frenich A Martínez Vidal JL Plaza Bolaños P 《Analytical and bioanalytical chemistry》2008,390(5):1413-1423
A multiresidue method for determining 22 polychlorinated biphenyls (PCBs) in air has been developed and validated by gas chromatography
(GC) coupled to tandem mass spectrometry (MS/MS) using a triple quadrupole analyzer (QqQ). The method was validated in terms
of both steps of sampling and analysis. The sampling method, which is based on active sampling using polyurethane foam (PUF)
as adsorbent, was validated by generating standard atmospheres. The retention capacity of this sampling sorbent allows up
to 5 m3 of air to be sampled without any breakthrough for most compounds. Two solvent extraction methods were compared: sonication
and Soxhlet extraction with a mixture of n-hexane:diethyl ether (95:5 v/v). Both extraction methods yielded similar results, but the first one required less solvent
and time. The method exhibited good accuracy (80.3–99.8%), precision (2.2–15.2%) and lower limits that allowed quantification
and confirmation at levels as low as 0.008 ng/m3. Finally, the method was applied to the analysis of PCBs in the air in areas near to a municipal solid-waste landfill and
directly above the refuse in the landfill, where it indicatedd the presence of some of the target compounds.
Figure General chemical structure of polychlorinated biphenyls 相似文献
11.
Francis Canon Franck Paté Emmanuelle Meudec Thérèse Marlin Véronique Cheynier Alexandre Giuliani Pascale Sarni-Manchado 《Analytical and bioanalytical chemistry》2009,395(8):2535-2545
Numerous protein–polyphenol interactions occur in biological and food domains particularly involving proline-rich proteins,
which are representative of the intrinsically unstructured protein group (IUP). Noncovalent protein–ligand complexes are readily
detected by electrospray ionization mass spectrometry (ESI-MS), which also gives access to ligand binding stoichiometry. Surprisingly,
the study of interactions between polyphenolic molecules and proteins is still an area where ESI-MS has poorly benefited,
whereas it has been extensively applied to the detection of noncovalent complexes. Electrospray ionization mass spectrometry
has been applied to the detection and the characterization of the complexes formed between tannins and a human salivary proline-rich
protein (PRP), namely IB5. The study of the complex stability was achieved by low-energy collision-induced dissociation (CID)
measurements, which are commonly implemented using triple quadrupole, hybrid quadrupole time-of-flight, or ion trap instruments.
Complexes composed of IB5 bound to a model polyphenol EgCG have been detected by ESI-MS and further analyzed by MS/MS. Mild
ESI interface conditions allowed us to observe intact noncovalent PRP–tannin complexes with stoichiometries ranging from 1:1
to 1:5. Thus, ESI-MS shows its efficiency for (1) the study of PRP–tannin interactions, (2) the determination of stoichiometry,
and (3) the study of complex stability. We were able to establish unambiguously both their stoichiometries and their overall
subunit architecture via tandem mass spectrometry and solution disruption experiments. Our results prove that IB5·EgCG complexes
are maintained intact in the gas phase.
相似文献
12.
Rodríguez-Fariñas N Gomez-Gomez MM Camara-Rica C 《Analytical and bioanalytical chemistry》2008,390(1):29-35
Oral administration of sodium tungstate is an effective treatment for type 1 and 2 diabetes in animal models; it does not
incur significant side effects, and it may constitute an alternative to insulin. However, the mechanism by which tungstate
exerts its observed metabolic effects in vivo is still not completely understood. In this work, serum-containing proteins
which bind tungstate have been characterized. Size exclusion chromatography (SEC) coupled to inductively coupled plasma mass
spectrometry (ICP-MS) with a Phenomenex Bio-Sep-S 2000 column and 20 mM HEPES and 150 mM NaCl at pH 7.4 as the mobile phase
was chosen as the most appropriate methodology to screen for tungsten–protein complexes. When human serum was incubated with
tungstate, three analytical peaks were observed, one related to tungstate–albumin binding, one to free tungstate, and one
to an unknown protein binding (MW higher than 300 kDa). Matrix-assisted laser desorption ionization time-of-flight (MALDI-TOF)
mass spectrometric analysis of the tungsten-containing fractions collected from SEC–ICP-MS chromatograms, after desalting
and preconcentration processes, confirmed the association of tungstate with albumin and the other unknown protein.
Figure SEC-ICP-MS // MALDI-TOF 相似文献
13.
Surmeian A Diplasu C Groza A Ganciu M Belenguer P Tempez A Chapon P 《Analytical and bioanalytical chemistry》2007,388(8):1625-1629
A high-current pulsed hollow cathode discharge was used to study the role of atomic and ionic metastables involved in ionization
plasma processes. We observed the enhancement of the spectral emission lines of noble gas ions in the afterglow. A study of
the processes that involve atomic and ionic metastables is of great interest since it should lead to a better understanding
of and enhanced control over the ionization mechanisms crucial to analytical glow discharge mass spectrometry (GDMS) analysis.
Figure Time profile of Ti, Ti+, and Ne+ spectral lines 相似文献
14.
Dumont E Ogra Y Vanhaecke F Suzuki KT Cornelis R 《Analytical and bioanalytical chemistry》2006,384(5):1196-1206
Liquid chromatography (LC) hyphenated with both elemental and molecular mass spectrometry has been used for Se speciation
in Se-enriched garlic. Different species were separated by ion-pair liquid chromatography–inductively coupled plasma mass
spectrometry (LC–ICP–MS) after hot-water extraction. They were identified by on-line reversed-phase liquid chromatography–electrospray
ionization tandem mass spectrometry (RPLC–ESI–MS–MS). Se-methionine and Se-methylselenocysteine were determined by monitoring
their product ions. Another compound, γ-glutamyl-Se-methylselenocysteine, shown to be the most abundant form of Se in the
garlic, was determined without any additional sample pre-treatment after extraction and without the need for a synthesized
standard. Product ions for this dipeptide were detected by LC–ESI–MS–MS for three isotopes of Se—78
Se, 80Se: and 82Se. The method was extended to the species extracted during in-vitro gastrointestinal digestion. Because both Se-methylselenocysteine
and γ-glutamyl-Se-methylselenocysteine have anticarcinogenic properties, their extractability and stability during human digestion
are very important. Garlic was also treated with saliva, to enable detection and analysis of species extracted during mastication.
Detailed information on the extractability of selenium species by both simulated gastric and intestinal fluid are given, and
variation of the distribution of Se among the different species with time is discussed. Although the main species in garlic
is the dipeptide γ-glutamyl-Se-methylselenocysteine, Se-methylselenocysteine is the main compound present in the extracts
after treatment with gastrointestinal fluids. Two more, so far unknown compounds were observed in the chromatogram. The extracted
species and their transformations were analysed by combining LC–ICP–MS and LC–ESI–MS–MS. In both the simulated gastric and
intestinal digests, Se-methionine, Se-methylselenocysteine, and γ-glutamyl-Se-methylselenocysteine could be determined by
LC–ESI–MS–MS by measuring their typical product ions.
相似文献
15.
Schütz K Persike M Carle R Schieber A 《Analytical and bioanalytical chemistry》2006,384(7-8):1511-1517
The anthocyanin pattern of artichoke heads (Cynara scolymus L.) has been investigated by high-performance liquid chromatography–electrospray ionization mass spectrometry. For this purpose a suitable extraction and liquid chromatographic method was developed. Besides the main anthocyanins—cyanidin 3,5-diglucoside, cyanidin 3-glucoside, cyanidin 3,5-malonyldiglucoside, cyanidin 3-(3′′-malonyl)glucoside, and cyanidin 3-(6′′-malonyl)glucoside—several minor compounds were identified. Among these, two peonidin derivatives and one delphinidin derivative were characterized on the basis of their fragmentation patterns. To the best of our knowledge this is the first report on anthocyanins in artichoke heads consisting of aglycones other than those of cyanidin. Quantification of individual compounds was performed by external calibration. Cyanidin 3-(6′′-malonyl)glucoside was found to be the major anthocyanin in all the samples analyzed. Total anthocyanin content ranged from 8.4 to 1,705.4 mg kg−1 dry mass.
相似文献
16.
Panuwet P Nguyen JV Kuklenyik P Udunka SO Needham LL Barr DB 《Analytical and bioanalytical chemistry》2008,391(5):1931-1939
We have developed a method using on-line solid-phase extraction–high-performance liquid chromatography–tandem mass spectrometry
(SPE-HPLC-MS/MS) and isotope dilution quantification to measure atrazine and seven atrazine metabolites in urine. The metabolites
measured were hydroxyatrazine, diaminochloroatrazine, desisopropylatrazine, desethylatrazine, desethylatrazine mercapturate,
atrazine mercaturate and atrazine itself. Our method has good precision (relative standard deviations ranging from 4 to 20%
at 5, 10 and 50 ng/mL), extraction efficiencies of 67 to 102% at 5 and 25 ng/mL, relative recoveries of 87 to 112% at 5, 25,
50 and 100 ng/mL limits of detection (LOD) ranging from 0.03 to 2.80 ng/mL. The linear range of our method spans from the
analyte LOD to 100 ng/mL (40 ng/mL for atrazine and atrazine mercapturate) with R
2 values of greater than 0.999 and errors about the slope of less than 3%. Our method is rapid, cost-effective and suitable
for large-scale sample analyses and is easily adaptable to other biological matrices. More importantly, this method will allow
us to better assess human exposure to atrazine-related chemicals.
Figure A schematic representation showing the elution of the analytes from the solid-phase extraction cartridge onto the analytical
column for chromatographic separation prior to MS/MS analysis 相似文献
17.
Various toxicological and metabolic interactions have been reported to exist between arsenic and selenium. In the present
study, synthetic seleno-arsenic compounds, potentially suitable for probing metabolic interactions between these two elements,
were prepared and tentatively characterized by using high-performance liquid chromatography (HPLC)–electrospray tandem mass
spectrometry and HPLC–inductively coupled plasma mass spectrometry. In analogy to the recently identified thio-arsenic species,
which can be prepared from their corresponding oxo-arsenic species via reaction with H2S, the seleno-arsenic compounds were also derived from oxo-arsenic compounds via reaction with H2Se.
Figure H2Se bubbled into solutions containing oxo‐arsenosugars converts them into their seleno‐arsenosugar analogues. 相似文献
18.
Careri M Costa A Elviri L Lagos JB Mangia A Terenghi M Cereti A Garoffo LP 《Analytical and bioanalytical chemistry》2007,389(6):1901-1907
A liquid chromatography–electrospray-tandem mass spectrometry (LC–ESI-MS–MS) method based on the detection of biomarker peptides
from allergenic proteins was devised for confirming and quantifying peanut allergens in foods. Peptides obtained from tryptic
digestion of Ara h 2 and Ara h 3/4 proteins were identified and characterized by LC–MS and LC–MS–MS with a quadrupole-time
of flight mass analyzer. Four peptides were chosen and investigated as biomarkers taking into account their selectivity, the
absence of missed cleavages, the uniform distribution in the Ara h 2 and Ara h 3/4 protein isoforms together with their spectral
features under ESI-MS–MS conditions, and good repeatability of LC retention time. Because of the different expression levels,
the selection of two different allergenic proteins was proved to be useful in the identification and univocal confirmation
of the presence of peanuts in foodstuffs. Using rice crispy and chocolate-based snacks as model food matrix, an LC–MS–MS method
with triple quadrupole mass analyzer allowed good detection limits to be obtained for Ara h2 (5 μg protein g−1 matrix) and Ara h3/4 (1 μg protein g−1 matrix). Linearity of the method was established in the 10–200 μg g−1 range of peanut proteins in the food matrix investigated. Method selectivity was demonstrated by analyzing tree nuts (almonds,
pecan nuts, hazelnuts, walnuts) and food ingredients such as milk, soy beans, chocolate, cornflakes, and rice crispy.
Figure ESI-QTOF-MS mass spectrum of Ara h3/4 triptig digest 相似文献
19.
Jahnke A Ahrens L Ebinghaus R Berger U Barber JL Temme C 《Analytical and bioanalytical chemistry》2007,387(3):965-975
This article describes the optimisation and validation of an analytical method for the determination of volatile polyfluorinated
alkyl substances (PFAS) in environmental air samples. Airborne fluorinated telomer alcohols (FTOHs) as well as fluorinated
sulfonamides and sulfonamidoethanols (FOSAs/FOSEs) were enriched on glass-fibre filters (GFFs), polyurethane foams (PUFs)
and XAD-2 resin by means of high-volume air samplers. Sensitive and selective determination was performed using gas chromatography/chemical
ionisation–mass spectrometry (GC/CI–MS). Five mass-labelled internal standard (IS) compounds were applied to ensure the accuracy
of the analytical results. No major blank problems were encountered. Recovery experiments were performed, showing losses of
the most volatile compounds during extraction and extract concentration as well as strong signal enhancement for FOSEs due
to matrix effects. Breakthrough experiments revealed losses of the most volatile FTOHs during sampling, while FOSAs/FOSEs
were quantitatively retained. Both analyte losses and matrix effects could be remediated by application of adequate mass-labelled
IS. Method quantification limits (MQLs) of the optimised method ranged from 0.2 to 2.5 pg/m3 for individual target compounds. As part of the method validation, an interlaboratory comparison of instrumental quantification
methods was conducted. The applicability of the method was demonstrated by means of environmental air samples from an urban
and a rural location in Northern Germany.
Figure High-volume air sampling of volatile polyfluorinated alkyl substances using glass fibre filters and PUF/XAD-2 cartridges at
a background monitoring site (Waldhof, Germany) 相似文献
20.
Liu Yang Shunjun Xu Chunjin Liu Zhijun Su 《Analytical and bioanalytical chemistry》2009,395(5):1441-1451
Ginsenoside Re is one of the major the bioactive triterpene saponins in ginseng root, a well-known adaptogen in traditional
Chinese medicine. It is believed that the lead compound may be further developed into a promising new drug for preventing
hypertension and cardiovascular disease. To better understand the pharmacological activities of the component, an investigation
of its in vivo metabolism was necessary. In the present study, a high-performance liquid chromatography coupled with electrospray
ionization and quadrupole time-of-flight tandem mass spectrometry (HPLC-ESI-TOF-MS/MS) has been applied to discover and identify
the metabolites of ginsenoside Re in rat urine following intravenous and oral administration of the component, respectively.
The rat urine samples were collected and pretreated through C18 solid-phase extraction cartridges prior to analysis. Negative electrospray ionization mass spectrometry was used to discern
ginsenoside Re and its possible metabolites in urine samples. The metabolites were identified and tentatively characterized
by means of comparing molecular mass, retention time, and fragmentation pattern of the analytes with those of the parent compound,
ginsenoside Re. As a result, eleven and nine metabolites together with Re were detected and identified in rat urine collected
after intravenous and oral administration, respectively. A possible metabolic pathway of ginsenoside Re was also investigated
and proposed. Oxidation and deglycosylation were found to be the major metabolic processes of the constituent in rat.
相似文献