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1.
Summary The chromatographic separation and resolution of the enantiomers of flurbiprofen and its two major metabolites, 4′-hydroxyflurbiprofen
and 3′-hydroxy-4′-methoxyflurbiprofen was investigated using four different approaches: reversed-phase HPLC after pre-column
derivatization with (R)-1-(naphthen-1-yl)ethylamine; reversed-phase HPLC using hydroxypropyl-β-cyclodextrin as a chiral mobile phase additive; chiral-phase
HPLC using either an α1-acid glycoprotein CSP (Chiral-AGP) or an amylose tris(3,5-dimethylphenylcarbamate) CSP (Chiralpak AD). Of all the approaches,
only the direct method using the Chiralpak AD CSP demonstrated separation and enantiomeric resolution of all three analytes
within an acceptable run time of 45 minutes. Enantiomeric resolution values of 1.67,3.67 and 3.44 were obtained for flurbiprofen,
4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen respectively. Semi-preparative isolation of the individual enantiomers
of both metabolites, followed by CD analysis, revealed that the elution order on the AD CSP wasR-beforeS-enantiomer for both metabolites and the same as that observed for flurbiprofen. The metabolite elution order was subsequently
confirmed on the analysis of urine samples obtained from a healthy volunteer following oral administration of the individual
drug enantiomers. 相似文献
2.
A reverse phase HPLC method was developed and validated for the simultaneous determination of 2-hydroxy-4-methoxybenzaldehyde
and 2-hydroxy-4-methoxybenzoic acid in the root extracts of Hemidesmus indicus. A comprehensive validation of the method including sensitivity, linearity, reproducibility, accuracy, limit of detection
(LOD) and limit of quantification (LOQ) was conducted using the optimized chromatographic conditions. The method was found
to be linear (r > 0.998) in the range of 5–350 μg mL−1 for 2-hydroxy-4-methoxybenzaldehyde and for 2-hydroxy-4-methoxybenzoic acid (r > 0.999) in the range 10–300 μg mL−1. The method was found to be precise with inter-day precision values (% RSD) in the ranges of 0.61–1.76% for 2-hydroxy-4-methoxybenzaldehyde
and 1.3–2.8% for 2-hydroxy-4-ethoxybenzoic acid while intra-day precisions (% RSD) of two analytes were in the range of 0.41–1.07
and 0.95–2.5%. The limits of detection (LODs) for 2-hydroxy-4-methoxybenzaldehyde and 2-hydroxy-4-methoxybenzoic acid were
0.84 and 2.34 μg mL−1. The described method was fast, sensitive and reproducible, and thus well suited for routine analysis of these two compounds
from root extracts of H. indicus and other plants. 相似文献
3.
A simple reversed-phase high-performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination
of the antiepileptic drugs (AEDs) zonisamide (ZNS), primidone (PRI), lamotrigine (LTG), phenobarbital (PB), phenytoin (PHT),
oxcarbazepine (OXC), and carbamazepine (CBZ) and two of their active metabolites, monohydroxycarbamazepine (MHD) and carbamazepine
10,11-epoxide (CBZE) in human plasma. Plasma (100 μL) was pretreated by deproteinization with 300 μL methanol containing 20 μg mL−1 propranolol hydrochloride as internal standard. HPLC was performed on a C8 column (4.6 mm × 250 mm; particle size 5 μm) with methanol–acetonitrile–0.1% trifluoroacetic acid, 235:120:645 (v/v), as mobile phase at a flow rate of 1.5 mL min−1. ZNS, OXC, and CBZ were monitored by UV detection at 235 nm, and PRI, LTG, MHD, PB, PHT, and CBZE by UV detection at 215 nm.
Relationships between response and concentration were linear over the concentration ranges 1–80 μg mL−1 for ZNS, 5–50 μg mL−1 for PRI, 1–25 μg mL−1 for LTG, 1–50 μg mL−1 for MHD, 5–100 μg mL−1 for PB, 1–10 μg mL−1 for CBZE, 0.5–25 μg mL−1 for OXC, 1–50 μg mL−1 for PHT, and 1–25 μg mL−1 for CBZ. Intra-day and inter-day reproducibility were adequate (coefficients of variation were ≤11.6%) and absolute recovery
ranged from 95.2 ± 6.13 to 107.7 ± 7.76% for all the analytes; for the IS recovery was 98.69 ± 1.12%. The method was proved
to be accurate, reproducible, convenient, and suitable for therapeutic monitoring of the nine analytes. 相似文献
4.
B. Venkateswara Reddy K. V. N. Suresh Reddy J. Sreeramulu G. V. Kanumula 《Chromatographia》2007,66(1-2):111-114
A rapid, specific reversed phase HPLC method has been developed for simultaneous determination of olanzapine and fluoxetine
in their formulations. Chromatographic separation of these two pharmaceuticals was carried out on an Inertsil C18 reversed phase column (150 mm × 4.6 mm, 5 μm) with a 40:30:30 (v/v/v) mixture of 9.5 mM sodium dihydrogen phosphate (pH adjusted to 6.8 ± 0.1 with triethylamine), acetonitrile and methanol as
mobile phase. The flow rate 1.2 mL min−1 and the analytes are monitored at 225 nm. Paroxetine was used as internal standard. The assay results were linear from 25
to 75 μg mL−1 for olanzapine (r
2 ≥ 0.995) and 100–300 μg mL−1 for fluoxetine (r
2 ≥ 0.995), showed intra- and inter-day precision less than 1.0%, and accuracy of 97.7–99.1% and 97.9–99.0%. LOQ was 0.005
and 0.001 μg mL−1 for olanzapine and fluoxetine, respectively. Separation was complete in less than 10 min. Validation of the method showed
it to be robust, precise, accurate and linear over the range of analysis. 相似文献
5.
Summary A reversed-phase ion-pair chromatographic (RPIPC) method withN,N,N′, N′-ethylenediaminetetrakis(methylenephosphonic acid) (EDTMP) as coordinating agent has been developed for simultaneous separation
and detection of Cu(II), Fe(III), and Pb(II) ions. Response is linearly dependent on amount of sample over the range 9.52–50.8
μg mL−1 for Cu(II), 8.31–41.8 μg mL−1 for Fe(III), and 37.3–51.8 μg mL−1 for Pb(II). The method has been applied successfully to an artificial mixed-ore sample. 相似文献
6.
Yan Liang Jie Sun Lin Xie An Kang Yuan Xie Wei-Dong Chen Hua Lv Guang-Ji Wang 《Chromatographia》2007,66(3-4):165-170
A sensitive and specific liquid chromatographic method with electrospray ionization mass spectrometry (LC–ESI-MS) has been
developed and validated for identification and quantification of mitiglinide in human urine. A simple liquid–liquid extraction
procedure was followed by separation on a C18 column with gradient elution, and detection using a single-quadrupole mass spectrometer in selected-ion-monitoring (SIM)
mode. The method was tested using six different batches of urine. Linearity was established for the mitiglinide concentrations
in the range 0.005–1.0 μg mL−1, with a coefficient of determination (r) of 0.9998 and good back-calculated accuracy and precision. Intra- and inter-day precision (as RSD, %) was below 10% and
accuracy for mitiglinide ranged from 85 to 115%. The lower limit of quantification was reproducible at 0.002 μg mL−1 for 500 μL urine. The proposed method enables unambiguous identification and quantification of mitiglinide in pre-clinical
and clinical studies. 相似文献
7.
Summary A clean method without use of organic solvents has been developed for isolation and high-performance liquid chromatographic
(HPLC) determination of oxytetracycline (OTC) and sulphadimidine (SDD) in cow's milk. Isolation is rapid and simple—homogenization
with an inorganic acid solution by means of a handy ultrasonic homogenizer, which is easy-to-use and portable, followed by
centrifugation. Reversed-phase HPLC was performed on a C4 column, with 1.25 mmol L−1 succinic acid solution as mobile phase, and identification was by means of a photodiode-array detector. Separation of the
analytes was achieved in less than 8 min. Significant linearity was established over the concentration range of 0.1–1.0 μg
mL−1 for both target compounds (r>0.99,P<0.01). Average recoveries of OTC and SDD (each spiked at 0.1–1.0 μg mL−1) were ≥88.8, and inter- and intra-assay variability was ≤2.8%. The total time required for analysis of one sample was <20
min. The limits of quantitation of the method (μg mL−1 in milk) were 0.044 for OTC and 0.023 for SDD. No organic solvent was used at any stage of the analysis. 相似文献
8.
A method for the simultaneous determination of N-methyl-2-pyrrolidone (NMP) and its metabolites 5-hydroxyl-N-pyrrolidone (5HNMP), N-methylsuccinimide (MSI) and 2-hydroxy-N-methylsuccinimide (2HMSI) in plasma and urine has been developed. Samples were purified by SPE using an ASPEC XL4. Analysis
was performed using LC–MS equipped with an APCI interface. The analysis provided linear responses in the range of 0.125–12 μg
mL−1 for all of the analytes and up to 150 μg mL−1 for 5HNMP and 2HMSI. The within day precision was in the range of 0.9–19.1% for plasma samples and 1.9–10.4% for urine samples
whereas the between day precisions were 4.5–11.9% and 1.2–17.5%, respectively. The method was deemed to be suitable for monitoring
the levels of NMP and its metabolites in the plasma and urine of occupationally exposed persons. 相似文献
9.
A simple, rapid and reproducible HPLC method was developed and validated for the simultaneous determination of olmesartan
(OLM) medoxomil and hydrochlorothiazide (HCT) in combined tablets. Chromatography was carried out on a 4.6 mm I.D × 200 mm,
5 μm cyano column with methanol–10 mM phosphoric acid containing 0.1% triethylamine (pH 2.5, 50:50 v/v) at a flow rate of 1.0 mL min−1 and UV detector was set at 260 nm. Valsartan (VAL) was used as internal standard (IS). A linear response was observed in the
range of 0.2–6 μg mL−1 (r
2 = 0.9998) for OLM and 0.1–4 μg mL−1 (r
2 = 0.9999) for HCT, respectively. The method showed good recoveries (99.56% for OLM and 99.48% for HCT) and the relative standard
deviation (RSD) values for intra- and inter-day precision were 0.70–1.59 and 0.80–2.00% for OLM and 1.20–1.37 and 1.63–1.93%
for HCT, respectively. The developed method was applied successfully for quality control assay of OLM and HCT in combined
tablets and in vitro dissolution studies. 相似文献
10.
Graziele P. Ramos Paula M. B. Dias Cláudia B. Morais Pedro E. Fröehlich Miguel Dall’Agnol José A. S. Zuanazzi 《Chromatographia》2008,67(1-2):125-129
Red clover (Trifolium pratense L.) is an important forage plant that contains the isoflavones daidzein, genistein, formononetin, and biochanin A. These
compounds have been studied lately due to their human health benefits. The aim of this study was to develop and validate an
HPLC method with simplified sample preparation to quantify daidzein, genistein, formononetin and biochanin A simultaneously
in red clover leaves. The validation showed that the method is specific, accurate, precise and robust, not to mention that
the sample preparation is easier and faster than those described earlier. The response was linear over a range of 0.01–0.2 μg mL−1 for daidzein, 0.05–0.5 μg mL−1 for genistein, 4–40 μg mL−1 for formononetin and 2–20 μg mL−1 for biochanin A. The range of recoveries was 85.6–101.0%. The RSD for intra- and inter-day precision were <2.54 and <7.22%,
respectively. Five populations of red clover, from the National Plant Germplasm System-USDA were analyzed and the content
of daidzein, genistein, formononetin and biochanin A ranged from 7.87–91.31, 51.60–131.30, 6568.33–23461.82, to 2499.55–10337.33 μg g−1 of dried material, respectively. 相似文献
11.
A high-performance liquid chromatography–UV method for determining DCJW concentration in rat plasma was developed. The method
described was applied to a pharmacokinetics study of intramuscular injection in rats. The plasma samples were deproteinized
with acetonitrile in a one-step extraction. The HPLC assay was carried out using a VP-ODS column and the mobile phase consisting
of acetonitrile–water (80:20, v/v) was used at a flow rate of 1.0 mL min−1 for the effective eluting DCJW. The detection of the analyte peak area was achieved by setting a UV detector at 314 nm with
no interfering plasma peak. The method was fully validated with the following validation parameters: linearity range 0.06–10 μg mL−1 (r > 0.999); absolute recoveries of DCJW were 97.44–103.46% from rat plasma; limit of quantification, 0.06 μg mL−1 and limit of detection, 0.02 μg mL−1. The method was further used to determine the concentration–time profiles of DCJW in the rat plasma following intramuscular
injection of DCJW solution at a dose of 1.2 mg kg−1. Maximum plasma concentration (C
max) and area under the plasma concentration–time curve (AUC) for DCJW were 140.20 ng mL−1 and 2405.28 ng h mL−1. 相似文献
12.
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
13.
A simple, rapid, and precise reversed-phase high-performance liquid chromatographic method has been developed for simultaneous determination of losartan potassium, ramipril, and hydrochlorothiazide. The three drugs were separated on a 150 mm × 4.6 mm i.d., 5 μm particle, Cosmosil C18 column. The mobile phase was 0.025 m sodium perchlorate–acetonitrile, 62:38 (v/v), containing 0.1% heptanesulphonic acid, pH adjusted to 2.85 with orthophosphoric acid, at a flow rate of 1.0 mL min−1. UV detection was performed at 215 nm. The method was validated for linearity, accuracy, precision, and limit of quantitation. Linearity, accuracy, and precision were acceptable in the ranges 35–65 μg mL−1 for losartan, 1.75–3.25 μg mL−1 for ramipril, and 8.75–16.25 μg mL−1 for hydrochlorothiazide. 相似文献
14.
Determination of triazine herbicides in human body fluids by solid-phase microextraction and capillary gas chromatography 总被引:2,自引:0,他引:2
T. Kumazawa X. -P. Lee K. Kondo K. Sato H. Seno K. Watanabe-Suzuki A. Ishii O. Suzuki 《Chromatographia》2000,52(3-4):195-199
Summary Eight triazine herbicides, prometon, propazine, atrazine, simazine, prometryn, ametryn, metribuzin, and cyanazine, have been
extracted from human whole blood and urine samples by headspace solid-phase microextraction (SPME) with a polydimethylsiloxane-coated
fiber and quantified by capillary gas chromatography with nitrogen-phosphorus detection.
Extraction efficiencies for all compounds were 0.21–0.99% for whole blood, except for cyanazine (0.06%). For urine, the extraction
efficiencies for prometon, propazine, atrazine, prometryn and ametryn were 13.6–38.1%, and those of simazine, metribuzin and
cyanazine were 1.35–8.73%.
The regression equations for the compounds extracted from whole blood were linear within the concentration ranged 0.01–1 μg
(0.5 mL)−1 for prometon, propazine, atrazine, prometryn, and ametryn, and 0.02–1 μg (0.5 mL)−1 for simazine, metribuzin, and cyanazine. For urine, regression equations for all compounds were linear within the concentration
range 0.005–0.25 μg mL−1. Compound detection limits were 2.8–9.0 ng (0.5 mL)−1 and 0.4–2.0 ng mL−1 for whole blood and urine, respectively. The coefficients of within-day and day-to-day variation were satisfactory for all
the compounds, and not greater than 10.3 and 14.2%, respectively.
Data obtained from determination of atrazine in rat whole blood after oral administration of the compound are also presented. 相似文献
15.
Lei Zhang Liang Xu Xiao-Jie Tan Qiong-Feng Liao Wei Guo Xiao-Hui Chen Kai-Shun Bi 《Chromatographia》2007,66(1-2):115-120
A sensitive and reliable ion-paired high-performance liquid chromatographic method has been established for the simultaneous
quantification of six major active ingredients, namely baicalin, baicalein, wogonin, oxysophocarpine, oxymatrine and matrine
in the Chinese herbal preparation, Sanwu-Huangqin-Tang. HPLC analyses were performed on a Phenomenex luna C18 column with mobile phase of methanol–acetonitrile–aqueous phosphoric acid at a flow rate of 0.9 mL min−1. The complete separation was achieved within 35 min for the six target constituents. A good linear regression relationship
between peak-areas and concentrations was obtained over the range of 12.10–242.0 μg*mL−1 for baicalin, 5.05–101.0 μg*mL−1 for baicalein, 0.95–19.0 μg*mL−1 for wogonin, 2.75–55.0 μg*mL−1 for oxysophocarpin, 2.75–55.0 μg*mL−1 for oxymatrine and 4.90–98.0 μg*mL−1 for matrine, respectively. The repeatability was evaluated by intra- and inter-day assays with relative standard deviation
(RSD) being less than 5.1%. The recoveries, measured at three concentration levels, varied from 93.8 to 102.1%. The assay
was successfully applied for determination of six bioactive compounds in Sanwu-Huangqin-Tang. The interaction of chemical
constituents was observed when the herbs were used in compatibility. The results indicated that the developed assay method
was rapid, accurate and could be readily utilized as a quality control method for Sanwu-Huangqin-Tang. 相似文献
16.
M. A. Campanero A. M. Zamarreño M. Simón M. C. Dios J. R. Azanza 《Chromatographia》1997,46(7-8):374-380
Summary A simple and rapid liquid chromatographic method has been developed for the determination of therapeutic levels of piperacillin
(I) and ceftazidime (II) in human plasma. Plasma and p-propionamidophenol (internal standard) were precipitated with methanol
(I) or 20% trichloroacetic acid (II). The supernatant was analysed on a 5 μm Spherisorb ODS C18 column with acetonitrile-0.05 M phosphate buffer pH 3.8 as mobile phase and ultraviolet detection at 254 nm. The calibration
graph was linear from 10 to 250 μg mL−1, for (I), and from 5 to 200 μg mL−1 for (II). Intra and inter-day CV did no exceed 2.29% for (I), and were 10.76–11.13%–2.00–5.62 for (II) at concentrations
of 10 μg mL−1 and 250 μg mL−1. 相似文献
17.
Summary A sensitive and rapid routine HPLC method is proposed for quantitative estimation of morphine hydrochloride and hydromorphone
hydrochloride in pharmaceutical dosage forms. The drugs were chromatographed on a C18 reversed-phase column; the mobile phase was acetonitrile-water, 35:65 (v/v), containing sodium dodecyl sulphate (0.5%, w/v),
as ion pairing reagent, and acetic acid (0.4% v/v). Detection was at 230 nm.
The optimized method was validated and linearity (r>0.999), precision, and accuracy were found to be acceptable within the concentration ranges 86–124 μg mL−1 for morphine hydroloride and 60–180 μg mL−1 for hydromorphone hydrochloride.
The method is being used to investigate the stability of morphine hydrochloride and hydromorphone hydrochloride in solution
used for intramuscular injection. 相似文献
18.
Haiyang Jiang Shuangyang Ding Fei Xu Sijun Zhao Jihong He Jinfeng Liu Xiaolin Hou Jianzhong Shen 《Chromatographia》2007,66(5-6):411-414
Eprinomectin is a novel and potent antiparasitic animal health drug. An analytical procedure for the determination of EPR
in bovine urine and feces has been developed. The urine sample was centrifuged and alkalized with ammonia following solid
phase extraction. The fecal sample was extracted with acetonitrile, defatted with hexane, cleaned-up using C18 cartridge.
All samples were analyzed by high performance liquid chromatography with fluorescence detection after derivatization with
N-methylimidazole. The limits of detection are 0.5 ng mL−1 and 0.5 ng g−1, respectively. Fortified at 2, 10, 50, and 100 ng mL−1(ng g−1), inter-assay recoveries of EPR in cattle urine and feces were in the range of 87.9–91.5% and 78.6–86.3%, with coefficients
of variation of 5.4–10.2% and 1.4–7.2%, respectively. Intra-assay mean recoveries of the analytes were 82.2–86.5% and 79.6–87.3%,
with coefficients of variation of 7.8–11.5% and 6.3–7.8%, respectively. The method was used to study the excretion of eprinomectin
in bovine urine and feces after subcutaneous administration at a dose of 0.5 mg kg−1. 相似文献
19.
A. M. Qandil B. M. Tashtoush B. M. Al-Taani S. M. Al-Nabulsi F. Al-Zogoul 《Chromatographia》2008,67(3-4):287-291
A simple, rapid and selective RP-HPLC method was developed and validated for the determination of ketorolac and five piperazinylalkyl
ester prodrugs. A binary isocratic mobile phase composed of a mixture of 65:35 (v/v) 0.02 M phosphate buffer (pH 5.4) and acetonitrile was used on a C18 column (125 × 4 mm, 5 μm). The injection volume was 25 μL and the detection wavelength was 314 nm and the flow rate was 1.5 mL min−1. The method exhibited excellent linearity with R
2 of no less than 0.999 and intra-assay and inter-assay precision that were less than the maximum amount allowed according
to Horwitz equation. The accuracy was found to be within the allowed ±15%. The limits of detection for the analytes were between
0.060 and 0.220 μg mL−1 and the limits of quantification were between 0.183 and 0.667 μg mL−1. This method was used successfully for the study of the solubility, stability and partition coefficients of piperazinylalkyl
ester prodrugs of ketorolac. 相似文献
20.
Determination of phenazopyridine in human plasma by high performance liquid chromatography 总被引:1,自引:0,他引:1
Summary A simple, low-cost, sensitive and selective HPLC method was developed for the determination of phenazopyridine in human plasma.
The method employs UV detection of phenazopyridine and of the internal Standard at 2 different wavelengths. Calibration curves
were linear over a large dynamic range, i.e., within 0.05–10.0 μg mL−1 with limit of quantification of 0.05 μg mL−1, and a limit of detection of 0.01 μg mL−1. 相似文献