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1.
Babu Rao Chandu Sreekanth Nama Kanchanamala Kanala Balasekhara Reddy Challa Rihana Parveen Shaik Mukkanti Khagga 《Analytical and bioanalytical chemistry》2010,398(3):1367-1374
A novel simple, sensitive, selective, and rapid high-performance liquid chromatography coupled with tandem mass spectrometry
method was developed and validated for quantification of riluzole in human plasma. The chromatography was performed by using
a Zorbax-SB-C18 (4.6 × 75 mm, 3.5 μm) column , isocratic mobile phase 0.1% formic acid/acetonitrile (10:90 v/v), and an isotope-labeled
internal standard (IS), [13C,15N2]riluzole. The extraction of drug and internal standard was performed by liquid–liquid extraction and analyzed by MS in the
multiple reaction monitoring (MRM) mode using the respective [M+H]+ ions, m/z 235.0/165.9 for riluzole and m/z 238.1/169.0 for the IS. The calibration curve was linear over the concentration range 0.5–500.0 ng/ml for riluzole in human
plasma. The limit of quantification (LOQ) was demonstrated at 0.5 ng/ml. The within-batch and between-batch precision were
0.6–2.3% and 1.4–5.7%, and accuracy was 97.1–101.1% and 98.8–101.2% for riluzole respectively. Drug and IS were eluted within
3.0 min. The validated method was successfully applied in a bioequivalence study of riluzole in human plasma. 相似文献
2.
An approach for rapid quantitation of 5-hydroxymethylfurfural (HMF) in honey using planar chromatography is suggested for
the first time. In high-performance thin-layer chromatography (HPTLC) the migration time is approximately 5 min. Detection
is performed by absorbance measurement at 290 nm. Polynomial calibration in the matrix over a range of 1:80 showed correlation
coefficients, r, of ≥ 0.9997 for peak areas and ≥ 0.9996 for peak heights. Repeatability in the matrix confirmed the suitability of HPTLC–UV
for quantitation of HMF in honey. The relative standard deviation (RSD, %, n = 6) of HMF at 10 ng/band was 2.9% (peak height) and 5.2% (peak area); it was 0.6% and 1.0%, respectively, at 100 ng/band.
Other possible detection modes, for example fluorescence measurement after post-chromatographic derivatization and mass spectrometric
detection, were also evaluated and can coupling can be used as an additional tool when it is necessary to confirm the results
of prior quantitation by HPTLC–UV. The confirmation is provided by monitoring the HMF sodium adduct [M + Na]+ at m/z 149 followed by quantitation in TIC or SIM mode. Detection limits for HPTLC–UV, HPTLC–MS (TIC), and HPTLC–MS (SIM) were 0.8 ng/band,
4 ng/band, and 0.9 ng/band, respectively. If 12 μL honey solution was applied to an HPTLC plate, the respective detection
limits for HMF in honey corresponded to 0.6 mg kg−1. Thus, the developed method was highly suitable for quantitation of HMF in honey at the strictest regulated level of 15 mg kg−1. Comparison of HPTLC–UV detection with HPTLC–MS showed findings were comparable, with a mean deviation of 5.1 mg kg−1 for quantitation in SIM mode and 6.1 mg kg−1 for quantitation in TIC mode. The mean deviation of the HPTLC method compared with the HPLC method was 0.9 mg kg-1 HMF in honey. Re-evaluation of the same HPTLC plate after one month showed a deviation of 0.5 mg kg−1 HMF in honey. It was demonstrated that the proposed HPTLC method is an effective method for HMF quantitation in honey.
相似文献
3.
Authors developed a simple, sensitive, selective, rapid, rugged, and reproducible liquid chromatography–tandem mass spectrometry
method for the quantification of eletriptan (EP) in human plasma using naratriptan (NP) as an internal standard (IS). Chromatographic
separation was performed on Ascentis Express C18, 50 × 4.6 mm, 2.7 μm column. Mobile phase was composed of 0.1% formic acid:
methanol (40:60 v/v), with 0.5 mL/min flow rate. Drug and IS were extracted by liquid–liquid extraction. EP and NP were detected with proton
adducts at m/z 383.2→84.3 and 336.2→97.8 in multiple reaction monitoring (MRM) positive mode, respectively. The method was validated with
the correlation coefficients of (r
2) ≥ 0.9963 over a linear concentration range of 0.5–250.0 ng/mL. This method demonstrated intra- and inter-day precision within
1.4–9.2% and 4.4–5.5% and accuracy within 96.8–103% and 98.5–99.8% for EP. This method is successfully applied in the bioequivalence
study of 24 human volunteers. 相似文献
4.
Benzylpiperazine (BZP) is an amphetamine-type stimulant, which was legally available in New Zealand and widely used in “Party
Pills” until reclassification as a Class C drug in April 2008. BZP was included as part of a multi-analyte method developed
for hair screening using high-performance liquid chromatography triple quadrupole mass spectrometry (LC-MS/MS). A 20-mg sample
of hair is extracted and partially purified using mixed-mode solid-phase extraction cartridges prior to analysis by LC-MS/MS.
The method was developed as a broad screen for drugs of abuse (including amphetamines, opiates, and benzodiazepines), with
only the BZP results being presented here. The assay was validated and found to be linear over the range of 0.085 to 8.65 ng/mg
with correlation coefficient of r
2 ≥ 0.99. Blank hair samples spiked with BZP at 0.22 and 2.16 ng/mg gave intra- and inter-day precision coefficients of variation
of ≤10% (n = 6 per day, 3 days) at both levels and calculated extraction efficiencies of 78% and 91%, respectively. The results from
the samples submitted to the laboratory for BZP analysis showed 11% were positive (n = 126). The mean BZP level was 3.9 ng/mg (range, 0.4–33 ng/mg; the result was extrapolated when above the calibration). These
data are the first available showing the levels expected from users of BZP. 相似文献
5.
Clavijo CF Hoffman KL Thomas JJ Carvalho B Chu LF Drover DR Hammer GB Christians U Galinkin JL 《Analytical and bioanalytical chemistry》2011,400(3):715-728
Opioids such as morphine are the cornerstone of pain treatment. The challenge of measuring the concentrations of morphine
and its active metabolites in order to assess human pharmacokinetics and monitor therapeutic drugs in children requires assays
with high sensitivity in small blood volumes. We developed and validated a semi-automated LC-MS/MS assay for the simultaneous
quantification of morphine and its active metabolites morphine 3β-glucuronide (M3G) and morphine 6β-glucuronide (M6G) in human
plasma and in dried blood spots (DBS). Reconstitution in water (DBS only) and addition of a protein precipitation solution
containing the internal standards were the only manual steps. Morphine and its metabolites were separated on a Kinetex 2.6-μm
PFP analytical column using an acetonitrile/0.1% formic acid gradient. The analytes were detected in the positive multiple
reaction mode. In plasma, the assay had the following performance characteristics: range of reliable response of 0.25–1000 ng/mL
(r
2 > 0.99) for morphine, 1–1,000 ng/mL (r
2 > 0.99) for M3G, and 2.5–1,000 ng/mL for M6G. In DBS, the assay had a range of reliable response of 1–1,000 ng/mL (r
2 > 0.99) for morphine and M3G, and of 2.5–1,000 ng/mL for M6G. For inter-day accuracy and precision for morphine, M3G and
M6G were within 15% of the nominal values in both plasma and DBS. There was no carryover, ion suppression, or matrix interferences.
The assay fulfilled all predefined acceptance criteria, and its sensitivity using DBS samples was adequate for the measurement
of pediatric pharmacokinetic samples using a small blood of only 20–50 μL. 相似文献
6.
Borges KB de Oliveira AR Barth T Jabor VA Pupo MT Bonato PS 《Analytical and bioanalytical chemistry》2011,399(2):915-925
The purpose of this study was the development and validation of an LC–MS–MS method for simultaneous analysis of ibuprofen
(IBP), 2-hydroxyibuprofen (2-OH-IBP) enantiomers, and carboxyibuprofen (COOH-IBP) stereoisomers in fungi culture medium, to
investigate the ability of some endophytic fungi to biotransform the chiral drug IBP into its metabolites. Resolution of IBP
and the stereoisomers of its main metabolites was achieved by use of a Chiralpak AS-H column (150 × 4.6 mm, 5 μm particle
size), column temperature 8 °C, and the mobile phase hexane–isopropanol–trifluoroacetic acid (95: 5: 0.1, v/v) at a flow rate of 1.2 mL min−1. Post-column infusion with 10 mmol L−1 ammonium acetate in methanol at a flow rate of 0.3 mL min−1 was performed to enhance MS detection (positive electrospray ionization). Liquid–liquid extraction was used for sample preparation
with hexane–ethyl acetate (1:1, v/v) as extraction solvent. Linearity was obtained in the range 0.1–20 μg mL−1 for IBP, 0.05–7.5 μg mL−1 for each 2-OH-IBP enantiomer, and 0.025–5.0 μg mL−1 for each COOH-IBP stereoisomer (r ≥ 0.99). The coefficients of variation and relative errors obtained in precision and accuracy studies (within-day and between-day)
were below 15%. The stability studies showed that the samples were stable (p > 0.05) during freeze and thaw cycles, short-term exposure to room temperature, storage at −20 °C, and biotransformation
conditions. Among the six fungi studied, only the strains Nigrospora sphaerica (SS67) and Chaetomium globosum (VR10) biotransformed IBP enantioselectively, with greater formation of the metabolite (+)-(S)-2-OH-IBP. Formation of the COOH-IBP stereoisomers, which involves hydroxylation at C3 and further oxidation to form the
carboxyl group, was not observed. 相似文献
7.
A simple and sensitive assay was developed and validated for the simultaneous quantification of rosuvastatin acid (RST), rosuvastatin-5S-lactone (RST-LAC), and N-desmethyl rosuvastatin (DM-RST), in buffered human plasma using liquid chromatography–tandem mass spectrometry (LC-MS/MS).
All the three analytes and the corresponding deuterium-labeled (d6) internal standards were extracted from 50 μL of buffered
human plasma by protein precipitation. The analytes were chromatographically separated using a Zorbax-SB Phenyl column (2.1 mm × 100 mm,
3.5 μm). The mobile phase comprised of a gradient mixture of 0.1% v/v glacial acetic acid in 10% v/v methanol in water (solvent A) and 40% v/v methanol in acetonitrile (solvent B). The analytes were separated at baseline within 6.0 min using a flow rate of 0.35 mL/min.
Mass spectrometry detection was carried out in positive electrospray ionization mode. The calibration curves for all three
analytes were linear (R ≥ 0.9964, n = 3) over the concentration range of 0.1–100 ng/mL for RST and RST-LAC, and 0.5–100 ng/mL for DM-RST. Mean extraction recoveries
ranged within 88.0–106%. Intra- and inter-run mean percent accuracy were within 91.8–111% and percent imprecision was ≤15%.
Stability studies revealed that all the analytes were stable in matrix during bench-top (6 h on ice–water slurry), at the
end of three successive freeze and thaw cycles and at −80°C for 1 month. The method was successfully applied in a clinical
study to determine the concentrations of RST and the lactone metabolite over 12-h post-dose in patients who received a single
dose of rosuvastatin. 相似文献
8.
Macwan JS Ionita IA Dostalek M Akhlaghi F 《Analytical and bioanalytical chemistry》2011,400(2):423-433
The aim of the proposed work was to develop and validate a simple and sensitive assay for the analysis of atorvastatin (ATV)
acid, ortho- and para-hydroxy-ATV, ATV lactone, and ortho- and para-hydroxy-ATV lactone in human plasma using liquid chromatography-tandem mass spectrometry. All six analytes and corresponding
deuterium (d5)-labeled internal standards were extracted from 50 μL of human plasma by protein precipitation. The chromatographic
separation of analytes was achieved using a Zorbax-SB Phenyl column (2.1 mm × 100 mm, 3.5 μm). The mobile phase consisted
of a gradient mixture of 0.1% v/v glacial acetic acid in 10% v/v methanol in water (solvent A) and 40% v/v methanol in acetonitrile (solvent B). All analytes including ortho- and para-hydroxy metabolites were baseline-separated within 7.0 min using a flow rate of 0.35 mL/min. Mass spectrometry detection was
carried out in positive electrospray ionization mode, with multiple-reaction monitoring scan. The calibration curves for all
analytes were linear (R
2 ≥ 0.9975, n = 3) over the concentration range of 0.05–100 ng/mL and with lower limit of quantitation of 0.05 ng/mL. Mean extraction recoveries
ranged between 88.6–111%. Intra- and inter-run mean percent accuracy were between 85–115% and percent imprecision was ≤ 15%.
Stability studies revealed that ATV acid and lactone forms were stable in plasma during bench top (6 h on ice-water slurry),
at the end of three successive freeze and thaw cycles and at −80 °C for 3 months. The method was successfully applied in a
clinical study to determine concentrations of ATV and its metabolites over 12 h post-dose in patients receiving atorvastatin. 相似文献
9.
Radix Scrophulariae (Xuanshen) is one of the famous Chinese herbal medicines widely used to treat rheumatism, tussis, pharyngalgia, arthritis,
constipation, and conjunctival congestion. Harpagoside and cinnamic acid are the main bioactive components of Xuanshen. The
purpose of this study was to develop an HPLC–UV method for simultaneous determination of harpagoside and cinnamic acid in
rat plasma and investigate pharmacokinetic parameters of harpagoside and cinnamic acid after oral administration of Xuanshen
extract (760 mg kg−1). After addition of syringin as internal standard, the analytes were isolated from plasma by liquid–liquid extraction. Separation
was achieved on a Kromasil C18 column, and detection was by UV absorption at 272 nm. The described assay was validated in terms of linearity, accuracy,
precision, recovery, and limit of quantification according to the FDA validation guidelines. Calibration curves for both analytes
were linear with the coefficient of variation (r) for both was greater than 0.999. Accuracy for harpagoside and cinnamic acid ranged from 100.7–103.5% and 96.9–102.9%, respectively,
and precision for both analytes were less than 8.5%. The main pharmacokinetic parameters found for harpagoside and cinnamic
acid after oral infusion of Xuanshen extract were as follows: C
max 1488.7 ± 205.9 and 556.8 ± 94.2 ng mL−1, T
max 2.09 ± 0.31 and (1.48 ± 0.14 h, AUC0–24 10336.4 ± 1426.8 and 3653.1 ± 456.4 ng h mL−1, 11276.8 ± 1321.4 and 3704.5 ± 398.8 ng h mL−1, and t
1/2 4.9 ± 1.3 and 2.5 ± 0.9 h, respectively. These results indicated that the proposed method is simple, selective, and feasible
for pharmacokinetic study of Radix Scrophulariae extract in rats.
Figure Radix Scrophulariae 相似文献
10.
Li Y Dong F Liu X Xu J Li J Lu C Wang Y Zheng Y 《Analytical and bioanalytical chemistry》2011,400(9):3097-3107
A rapid and simple miniaturized liquid–liquid extraction method has been developed for the determination of topramezone in
soil, corn, wheat, and water samples using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-electrospray
ionization (ESI)/MS/MS). The established method for the extraction and purification procedure was based on liquid–liquid partitioning
into an aqueous solution at a low pH (pH ≈ 2.5), followed by back-partitioning into water at pH > 9. Two precursor, product
ion transitions for topramezone were measured and evaluated to provide the maximum degree of confidence in the results. Under
negative ESI conditions, quantitation was achieved by monitoring the fragment at m/z = 334 and the qualitative fragment at m/z = 318, whereas also collecting the corresponding parent ion at m/z = 362. Chromatographic separation was achieved using gradient elution with a mobile phase consisting of methanol and a 0.01%
aqueous ammonium hydroxide solution. Recovery studies for soil, corn, wheat, and water were conducted at four different topramezone
concentrations (5 or 10, 50, 100, and 1,000 μg kg−1); the overall average recoveries ranged from 79.9% to 98.4% with intra-day relative standard deviations (RSD) of 3.1~8.7%
and inter-day RSD of 4.3~7.5%. Quantitative results were determined from calibration curves of topramezone standards containing
1–500 μg L−1 with an R
2 ≥ 0.9994. Method sensitivities expressed as limits of quantitation were typically 6, 8, 9, and 1 μg kg−1 in soil, corn, wheat, and water, respectively. The results of the method validation confirmed that this proposed method was
convenient and reliable for the determination of topramezone residues in soil, corn, wheat, and water. 相似文献
11.
A liquid chromatography–mass spectrometry (LC-MS) method was developed and validated for the simultaneous determination of
alisol A and alisol A 24-acetate from Alisma orientale (Sam.) Juz. in rat plasma using diazepam as an internal standard. A 200-μl plasma sample was extracted by methyl tert-butyl ether and the separation was performed on Kromasil C18 column (150 × 4.6 mm, 5 μm) with the mobile phase of acetonitrile (containing 0.1% of formic acid)–water (73:27, v/v) at a flow rate of 0.8 ml/min in a run time of 10 min. The two analytes were monitored with positive electrospray ionization
by selected ion monitoring mode. The lower limit of quantitation for both alisol A and alisol A 24-acetate were 10 ng/ml.
The calibration curves were linear in the measured range 10–1,000 ng/ml for alisol A and 10–500 ng/ml for alisol A 24-acetate.
The mean extraction recoveries were above 74.7% for alisol A and above 72.4% for alisol A 24-acetate from biological matrixes.
The intra- and inter-day precision for all concentrations of quality controls was lower than 14.1% (RSD %) for each analyte.
The accuracy ranged from −12.3% to 9.8% (RE %) for alisol A, and −8.6% to 14.2% (RE %) for alisol A 24-acetate. The method
was successfully applied to the study on the pharmacokinetics of alisol A and alisol A 24-acetate in rat plasma. 相似文献
12.
An ultra-performance liquid chromatography-tandem mass spectrometry method was developed, optimised and validated for the
quantification of synthetic folic acid (FA), also called pteroyl-l-glutamic acid or vitamin B9 and naturally occurring 5-methyltetrahydrofolate (5-MTHF) found in folate-fortified breads. Optimised
sample preparation prior to analysis involved addition of 13C5 labelled internal standards, treatments with α-amylase and rat serum, solid-phase extraction using aromatic-selective cartridges
and ultra-filtration. Analytes were separated on a Waters ACQUITY HSS T3 column during a 6-min run and analysed by positive
ion electrospray selected reaction monitoring MS/MS. Standard calibration curves for the two analytes were linear over the
range of 0.018–14 μg FA/g of fresh bread (r
2 = 0.997) and 9.3–900 ng 5-MTHF/g of fresh bread (r
2 = 0.999). The absolute recoveries were 90% and 76% for FA and 5-MTHF, respectively. Intra-day coefficients of variation were
3% for FA and 18% for 5-MTHF. The limit of detection was 9.0 ng/g for FA and 4.3 ng/g for 5-MTHF, determined using pre-extracted
tapioca starch as the blank matrix. The assay is rugged, fast, accurate and sensitive, applicable to a variety of food matrices
and is capable of the detection and quantification of the naturally occurring low levels of 5-MTHF in wheat breads. The findings
of this study revealed that the FA range in Australian fortified breads was 79–110 μg/100 g of fresh bread and suggest that
the flour may not have the mandated FA fortification level (200–300 μg/100 g of flour), though this cannot be determined conclusively
from experimental bread data alone, as variable baking losses have been documented by other authors. 相似文献
13.
Davis C Gordon N Murphy S Singh I Kavanagh K Carberry S Doyle S 《Analytical and bioanalytical chemistry》2011,401(8):2519-2529
Gliotoxin is produced by non-ribosomal peptide synthesis and secreted from certain fungi, including Aspergillus fumigatus. It is an epipolythiodioxopiperazine that contains an intact disulphide bridge and is the focus of intense research as a
consequence of its negative immunomodulatory properties. Gliotoxin detection is generally enabled by reversed-phase–high-performance
liquid chromatography (RP-HPLC), with absorbance detection (220–280 nm), or liquid chromatography-mass spectrometry, yet detection
is not readily achievable by matrix-assisted laser desorption ionisation–time-of-flight mass spectrometry (MALDI-ToF MS).
We have developed a single-pot derivatisation strategy which uses sodium borohydride-mediated reduction of gliotoxin followed
by immediate alkylation of exposed thiols by 5′-iodoacetamidofluorescein to yield a stable product, diacetamidofluorescein-gliotoxin
(GT-(AF)2), of molecular mass 1103.931 Da ((M + H)+). This product is readily detectable by RP-HPLC and exhibits a 6.8-fold increase
in molar absorptivity compared with gliotoxin, which results in a higher sensitivity of detection (40 ng; 125 pmoL). GT-(AF)2 also fluoresces (excitation/emission, 492:518 nm). Unlike free gliotoxin, the product (>800 fmol) is detectable by MALDI-ToF
MS. Sporidesmin A can also be detected by RP-HPLC and MALDI-ToF MS (>530 fmol) using this strategy. We also demonstrate that
the strategy facilitates detection of gliotoxin (mean ± SD = 3.55 ± 0.07 μg 100 μL−1; n = 2) produced by A. fumigatus, without the requirement for organic extraction of culture supernatants and associated solvent removal. GT-(AF)2 is also detectable (150 ng; 460 pmol) by thin-layer chromatography. 相似文献
14.
A fast and sensitive liquid chromatography–mass spectrometry method was developed for the determination of ursolic acid (UA)
in rat plasma and tissues. Glycyrrhetinic acid was used as the internal standard (IS). Chromatographic separation was performed
on a 3.5 μm Zorbax SB-C18 column (30 mm × 2.1 mm) with a mobile phase consisting of methanol and aqueous 10 mM ammonium acetate
using gradient elution. Quantification was performed by selected ion monitoring with (m/z)− 455 for UA and (m/z)− 469 for the IS. The method was validated in the concentration range of 2.5 − 1470 ng mL−1 for plasma samples and 20 − 11760 ng g−1 for tissue homogenates. The intra- and inter-day assay of precision in plasma and tissues ranged from 1.6% to 7.1% and 3.7%
to 9.0%, respectively, and the intra- and inter-day assay accuracy was 84.2 − 106.9% and 82.1 − 108.1%, respectively. Recoveries
in plasma and tissues ranged from 83.2% to 106.2%. The limits of detections were 0.5 ng mL−1 or 4.0 ng g−1. The recoveries for all samples were >90%, except for liver, which indicated that ursolic acid may metabolize in liver. The
main pharmacokinetic parameters obtained were T
max = 0.42 ± 0.11 h, C
max = 1.10 ± 0.31 μg mL−1, AUC = 1.45 ± 0.21 μg h mL−1 and K
a = 5.64 ± 1.89 h−1. The concentrations of UA in rat lung, spleen, liver, heart, and cerebellum were studied for the first time. This method
is validated and could be applicable to the investigation of the pharmacokinetics and tissue distribution of UA in rats. 相似文献
15.
Moser C Zoderer D Luef G Rauchenzauner M Wildt L Griesmacher A Seger C 《Analytical and bioanalytical chemistry》2012,403(4):961-972
Co-administration of synthetic progestin containing hormonal contraceptives (HCs) and antiepileptic drugs (AEDs) is a common
clinical situation which needs specific considerations due to drug interactions. Several studies have demonstrated that lamotrigine
plasma levels are significantly decreased during co-medication with HCs, and that this interaction is associated with increased
seizure frequency in most of the cases. Additionally, an increase in contraceptive failure and unintended pregnancy could
be observed during co-medication. Hence, monitoring of progestin plasma levels in patients with AED co-medication is of interest.
A rapid and reliable online solid-phase extraction-high performance liquid chromatography–tandem mass spectrometry (online
SPE-LC-MS/MS) method using gradient elution in the LC domain was established and validated for the simultaneous quantitative
determination of gestodene, dienogest, drospirenone, etonogestrel, cyproterone acetate, and levonorgestrel in human plasma.
The online SPE-LC-MS/MS method covered a quantification concentration range of 5–100 ng/ml for dienogest, 1–100 ng/ml for
etonogestrel and 2–100 ng/ml for all other analytes. Stable isotope-labeled internal standards were used for analyte quantification
based on selected reaction monitoring experiments. Inter- and intra-assay precision and accuracy were determined from quality
control (QC) samples at the lower limits of quantification and at low, medium, and high concentration levels within the calibration
range. Inter-assay reproducibility at the QC levels was better than 10% (relative standard deviation, RSD), accuracy at these
levels ranged from −3.7% to 11.3%. Total extraction efficiency, tested at three concentrations, ranged from 92.5% to 106.4%.
Matrix interferences were excluded by post-column infusion experiments. To prove the applicability of the assay in clinical
cohorts, a sample set (n = 298) stemming from study patients under AED/oral HC co-medication was screened for progestin plasma levels. This method
has to be considered a research-use-only assay and must not be used for diagnostic or therapeutic purposes, since it did not
undergo formal performance evaluation in the sense of the IVD directive (98/79/EG) of the European Community. 相似文献
16.
Laura Luosujärvi Markus Haapala Mario Thevis Ville Saarela Sami Franssila Raimo A. Ketola Risto Kostiainen Tapio Kotiaho 《Journal of the American Society for Mass Spectrometry》2010,21(2):310-316
A gas chromatography-microchip atmospheric pressure photoionization-mass spectrometric (GC-μAPPI-MS) method was developed and used for the analysis of three 2-quinolinone-derived selective androgen receptor modulators
(SARMs). SARMs were analyzed from spiked urine samples, which were hydrolyzed and derivatized with N-methyl-N-(trimethylsilyl)trifluoroacetamide before analysis. Trimethylsilyl derivatives of SARMs formed both radical cations (M+•) and protonated molecules ([M + H]+) in photoionization. Better signal-to-noise ratios (S/N) were obtained in MS/MS analysis using the M+• ions as precursor ions than using the [M + H]+ ions, and therefore the M+• ions were selected for the precursor ions in selected reaction monitoring (SRM) analysis. Limits of detection (LODs) with
the method ranged from 0.01 to 1 ng/mL, which correspond to instrumental LODs of 0.2–20 pg. Limits of quantitation ranged
from 0.03 to 3 ng/mL. The mass spectrometric response to the analytes was linear (R ≥ 0.995) from the LOQ concentration level
up to 100 ng/mL concentration, and intra-day repeatabilities were 5%–9%. In addition to the GC-μAPPI-MS study, the proof-of-principle of gas chromatography-microchip atmospheric pressure chemical ionization-Orbitrap MS
(GC-μAPCI-Orbitrap MS) was demonstrated. 相似文献
17.
Li C Wen D Zhang J Chen Z Cong W Rao Z Liu H 《Analytical and bioanalytical chemistry》2006,386(7-8):1985-1993
Metabolism of four tobacco-specific N-nitrosamines (TSNAs), N′-nitrosonornicotine (NNN), N′-nitrosoanatabine (NAT), N′-nitrosoanabasine (NAB), and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) has been studied by solid-phase extraction
(SPE) and liquid chromatography–tandem mass spectrometry (LC–MS–MS). 4-(Methylnitrosamino)-4-(3-pyridyl)-1-butanol (iso-NNAL)
was used as internal standard. SPE and LC–MS–MS was found to be a rapid, simple, sensitive, and selective method for analysis
of TSNAs in rabbit serum. The relative standard deviation (R.S.D., n = 6) for analysis of 5 ng mL−1 and 0.5 ng mL−1 standards and of serum sample spiked with 5 ng mL−1 standards of five TSNAs was 2.1–11% and recovery of 5 ng mL−1 standards from serum was 100.2–112.9%. A good linear relationship was obtained between peak area ratio and concentration
in the range of 0.2–100 ng mL−1 for NNAL and 0.5–100 ng mL−1 for other four TSNAs, with correlation coefficients (R
2) >0.99 (both linear and log–log regression). Detection limits for standards in solvent were between 0.04 and 0.10 ng mL−1. Doses of TSNAs administered to rabbits via the auricular vein were 4.67 μg kg−1 and 11.67 μg kg−1, in accordance with the different levels in cigarettes. Metabolic curves were obtained for the four TSNAs and for 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol
(NNAL), a metabolite of NNK; on the basis of these curves we modeled metabolic kinetic equations for these TSNAs by nonlinear
curve fitting. 相似文献
18.
Wilhelmina H. A. de Jong Marianne H. L. I. Wilkens Elisabeth G. E. de Vries Ido P. Kema 《Analytical and bioanalytical chemistry》2010,396(7):2609-2616
Serotonin emerges as crucial neurotransmitter and hormone in a growing number of different physiologic processes. Besides
extensive serotonin production previously noted in patients with metastatic carcinoid tumors, serotonin now is implicated
in liver cell regeneration and bone formation. The aim was to develop a rapid, sensitive, and highly selective automated on-line
solid-phase extraction method coupled to high-performance liquid chromatography–tandem mass spectrometry (XLC-MS/MS) to quantify
low serotonin concentrations in matrices such as platelet-poor plasma and urine. Fifty microliters plasma or 2.5 μL urine
equivalent were pre-purified by automated on-line solid-phase extraction, using weak cation exchange. Chromatography of serotonin
and its deuterated internal standard was performed with hydrophilic interaction chromatography. Mass spectrometric detection
was operated in multiple reaction monitoring mode using a quadrupole tandem mass spectrometer with positive electrospray ionization.
Serotonin concentrations were determined in platelet-poor plasma of metastatic carcinoid patients (n = 23) and healthy controls (n = 22). Urinary reference intervals were set by analyzing 24-h urine collections of 120 healthy subjects. Total run-time was
6 min. Intra- and inter-assay analytical variation were <10%. Linearity in the 0–7300 μmol/L calibration range was excellent
(R2 > 0.99). Quantification limits were 30 and 0.9 nmol/L in urine and plasma, respectively. Platelet-poor serotonin concentrations
in metastatic carcinoid patients were significantly higher than in controls. The urinary reference interval was 10–78 μmol/mol
creatinine. Serotonin analysis with sensitive and specific XLC-MS/MS overcomes limitations of conventional HPLC. This enables
accurate quantification of serotonin for both routine diagnostic procedures and research in serotonin-related disorders. 相似文献
19.
This study presents a high-performance liquid chromatography–electrospray ionization–mass spectrometric (LC–ESI–MS) method
for the simultaneous determination of tramadol and acetaminophen in human plasma using phenacetinum as the internal standard.
After alkalization with saturated sodium bicarbonate, both compounds were extracted from human plasma with ethyl acetate and
were separated by HPLC on a Hanbon LiChrospher CN column with a mobile phase of 10 mM ammonium acetate buffer containing 0.5%
formic acid–methanol (40:60, v/v) at a flow rate of 1 mL min−1. Analytes were determined using electrospray ionization in a single quadrupole mass spectrometer. LC–ESI–MS was performed
in the positive selected-ion monitoring (SIM) mode using target ions at [M+H]+
m/z 264.3 for tramadol, [M+H]+
m/z 152.2 for acetaminophen and [M+H]+
m/z 180.2 for phenacetinum. Calibration curves were linear over the range of 5–600 ng mL−1 for tramadol and 0.03–16 μg mL−1 for acetaminophen. The inter-run relative standard deviations were less than 14.4% for tramadol and 12.3% for acetaminophen.
The intra-run relative standard deviations were less than 9.3% for tramadol and 7.9% for acetaminophen. The mean plasma extraction
recovery for tramadol and acetaminophen were in the ranges of 82.7–85.9 and 83.6–85.3%. The method was applied to study the
pharmacokinetics of a new formulation of tramadol/acetaminophen tablet in healthy Chinese volunteers. 相似文献
20.
Summary Direct chiral-phase HPLC methods have been developed for the determination of flurbiprofen and its major metabolites, namely
4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen, in biological fluids using a derivatized amylose chiral stationary
phase (CSP; Chiral-pak AD). Quantification of all three analytes, both free and conjugated, in urine was carried out following
liquid-liquid extraction using tandem ultraviolet (UV) and fluorescence detection. Determination of flurbiprofen and the 4′-hydroxy-metabolite
in plasma utilized the same CSP but required modification in the mobile phase composition and sole use of fluorescence detection.
The urine assay was linear (r>0.998) between 0.05–10 μg mL−1, 0.1–20 μg mL−1 and 0.01–2 μg mL−1 for the enantiomers of flurbiprofen, 4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen respectively. The plasma
assay was linear (r>0.997) between 0.1–6 μg mL−1 and 0.01–0.6 μg mL−1 for the enantiomers of flurbiprofen and 4′-hydroxyflurbiprofen respectively. Both assays, typically yielded within- and between-day
imprecision and accuracy values less than 10% for the enantiomers of the different analytes. Initial volunteer studies suggest
that the disposition of flurbiprofen displays modest enantioselectivity in humans. 相似文献