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71.
Girault J. Longueville D. Malgouyat J. M. Istin B. Lecomte G. Fourtillan J. B. 《Chromatographia》1994,39(3-4):228-238
Summary A simple and sensitive assay has been developed for the quantitative measurement of a new platelet activating factor antagonist (BN50730), and its two main metabolites (BN50727 and BN50922), at the picomole level in human plasma and urine. The three compounds of interest and the internal standard (BN50765) were measured by combined LC-negative chemical ionization MS. A simple solid-liquid extraction procedure was used to isolate the parent drug and the two metabolites. The MS was tuned to monitor the intense ionm/z 333 generated in the ion source by a dissociative capture process. The assay was on 1 ml plasma or 0.1 ml urine and the quantitation limit was calculated as 1 ng·ml–1. The very low relative standard deviations and mean percentages of error calculated for within-day or between-day repeatability assays demonstrate the ruggedness of the technique for routine determination in biological fluids. Some preliminary results on the pharmacokinetics of the parent drug and its two main metabolites illustrate the applicability of this method. 相似文献
72.
Sun Y Irie M Kishikawa N Wada M Kuroda N Nakashima K 《Biomedical chromatography : BMC》2004,18(8):501-507
A highly sensitive HPLC method was developed for the determination of xenoestrogenic compound, bisphenol A (BPA) in human breast milk samples. After a two-step liquid-liquid extraction, BPA was derivatized with fluorescent labeling reagent, 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl). The excess fluorescent reagent could be removed effectively using a column-switching system. The separation of DIB-BPA from endogenous materials in milk was carried out on two C(18) columns and fluorescence intensity was monitored at 475 nm with the excitation of 350 nm. A good linearity (r = 0.994) was observed of BPA in the concentration range of 0.2-5.0 ng mL(-1) in breast milk, and the detection limit was 0.11 ng mL(-1) at a signal-to-noise ratio of 3. Intra- and inter-day precision (RSD, %) were less than 8.7 and 10.4, respectively. Twenty-three breast milk samples of healthy lactating women were analyzed for the BPA concentration; the mean value was 0.61 +/- 0.20 ng mL(-1), with no correlation to the lipid content of milk samples. 相似文献
73.
食物中的钼与人体健康 总被引:5,自引:0,他引:5
综述了食物中钼与人体健康之间的关系.主要包括常见食物中的钼含量,钼在人体中的代谢,钼的生物学功能以及钼对人体健康的影响等. 相似文献
74.
Pinto FG Andrada D Magalhães CG Nunes BR de Amorim FR Franco MB Saint'pierre TD da Silva JB Curtius AJ 《Analytical and bioanalytical chemistry》2005,383(5):825-832
Different chemical modifiers for use with electrothermal atomic absorption spectrometry (ET AAS) were investigated in relation
to determining the selenium in human urine samples. The samples were diluted in a solution containing 1% v/v HNO3 and 0.02% m/v cetyltrimethylammonium chloride (CTAC). Studying the modifiers showed that the use of either Ru or Ir as the
permanent modifier gave low sensitivity to Se and the peak shape was very noisy, while Zr or Rh gave no peak at all. The same
occurred when Zr was used in solution. For mixtures of permanent modifiers, Ir plus Rh or Zr plus Rh gave very low sensitivity,
Zr plus Rh with co-injection of Ir in solution was also not efficient, Zr plus Rh in solution gave good sensitivity, but the
best results were obtained with a mixture of Zr and Rh as the permanent modifier and co-injection of Rh in solution. Using
this last modifier, the following dilutions with the HNO3 and CTAC were studied: 1:1, 1:2, 1:3 and 1:4. The best dilution was 1:1, which promoted good sensitivity and a more defined
peak shape and made it possible to correct for the background using a deuterium arc lamp. Under these conditions, a characteristic
mass of 26±0.2 pg was obtained for Se in aqueous solution. Six certified urine samples were analyzed using matrix matching
calibration and the measured concentrations were in agreement with the certified values, according to a t-test at the 95%
confidence level. Recovery tests were carried out and the recoveries were in the range 100–103%, with relative standard deviation
better than 9%. The limit of detection (LOD, 3 sd, n=10) was 3.0 μg L−1 in the sample. The treated graphite tube could be used for at least 600 atomization cycles without significant alteration
of the analytical signal. 相似文献
75.
Summary The native enantioselectivity in binding of human serum albumin (HSA) towards 2-aryl propionic acid non-steroidal anti-inflammatory drugs (2-APA-NSAIDs, the profens) was found to be preserved when the protein was immobilized within a commercially available diol high-performance liquid chromatographic column. High capacity factors were obtained, reflecting the previously observed extensive binding of the 2-APA-NSAIDs to free HSA. The capacity factors were modified by the addition of octanoic acid to the mobile phase. Chiral resolution of the enantiomers of all nine 2-APA-NSAIDs studied was achieved. Preliminary studies show that in addition to being a useful chiral analytical tool for this therapeutically important series of compounds, the HSA chiral stationary phase may provide useful information on the affinity and binding mechanism of small molecules to HSA. 相似文献
76.
Summary A rapid and efficient procedure is described for extraction and determination of aminocaproic acid in horse urine. Urine was
extracted by passing through a bonded silica column (Bond-Elut). The adsorbed drug was washed free of endogenous materials
before being eluted. The extract was then examined by thin-layer chromatography and HPLC. The purity of the extract was determined
by gas chromatography-mass spectrometry. 相似文献
77.
The use of a laboratory-made iodide ion-selective electrode with tubular configuration and based on a crystalline membrane (AgI/Ag2S) as the detector for ion chromatographic determination of iodide in urine and serum is described. A CIS reversed-phase column was coated withN-cetylpyridinium chloride to prepare a low-exchange-capacity analytical column and with hexadecyltrimethylammonium bromide to prepare a concentrator pre-column. A 2.0 ml min–1 flow rate of deionized water and 0.1 mol 1–1 KNO3 solution was used for the pre-concentration and for the chromatographic separation, respectively. For optimum performance of the detector a background level of iodide was added into the column effluent. A linear relationship (r = 0.9997) between tubular electrode potential (as peak height) and iodide concentration in the range 5–400 g 1–1 and a detection limit of 1.47 g 1–1 were obtained. The method shows good reproducibility for both peak height (2.2% RSD) and retention time (1.3% RSD). Recoveries on its application to the samples were 93.0–100.9% for urine and 91.4–106.0% for serum. 相似文献
78.
Rodríguez Flores J Berzas Nevado JJ Durán Merás I Rodríguez Gómez MJ 《Journal of separation science》2005,28(7):658-664
A capillary zone electrophoresis (CZE) method using a fused-silica capillary (60.2 cm x 75 microm ID) was investigated for the determination of triamterene (TRI), methotrexate (MTX), and creatinine (CREA) in human urine. The separation was performed using a hydrodynamic injection time of 7 s (0.5 psi), a voltage of 25 kV, a capillary temperature of 30 degrees C, and 40 mM phosphoric acid adjusted to pH 2.25 by addition of triethanolamine as separation electrolyte. Under these conditions, analysis takes about 15 min. A linear response over the 0.5-15.0 mg L(-1) concentration range was found for TRI and MTX, and 0.5-80.0 mg L(-1) for CREA. Dilution of the sample (water:urine, 1:1 for TRI and MTX, and 1:25 for CREA determination) was the only step necessary prior to analysis by electrophoresis. The developed method is easy, rapid, and sensitive and has been applied to determine triamterene,methotrexate, and creatinine in urine samples with satisfactory results. 相似文献
79.
Studies are described on the phase I and II metabolism and the toxicological analysis of the piperazine-derived designer drug 1-(3-trifluoromethylphenyl)piperazine (TFMPP) in rat urine using gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS). The identified metabolites indicated that TFMPP was extensively metabolized, mainly by hydroxylation of the aromatic ring and by degradation of the piperazine moiety to N-(3-trifluoromethylphenyl)ethylenediamine, N-(hydroxy-3-trifluoromethylphenyl)ethylenediamine, 3-trifluoromethylaniline, and hydroxy-3-trifluoromethylaniline. Phase II reactions included glucuronidation, sulfatation and acetylation of phase I metabolites. The authors' systematic toxicological analysis (STA) procedure using full-scan GC/MS after acid hydrolysis, liquid-liquid extraction and microwave-assisted acetylation allowed the detection of TFMPP and its above-mentioned metabolites in rat urine after single administration of a dose calculated from the doses commonly taken by drug users. Assuming similar metabolism, the described STA procedure should be suitable for proof of an intake of TFMPP in human urine. 相似文献
80.