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1.
A stability-indicating LC method was developed for the simultaneous determination of ibuprofen and diphenhydramine citrate in pharmaceutical dosage forms. The chromatographic separation was achieved on an Inertsil ODS 3V, 150 × 4.6 mm, 5 μm, column. The mobile phase contained a mixture of 50 mM potassium dihydrogen phosphate buffer:acetonitrile:triethylamine:glacial acetic acid (55:45:0.2:0.2, v/v/v/v). This method allowed the determination of 2.85–9.14 mg mL?1 of ibuprofen and 0.54–1.73 mg mL?1 of diphenhydramine citrate, in a diluent consisting of pH 7.2, 50 mM potassium dihydrogen phosphate buffer:acetonitrile (40:60, v/v). The flow rate was 1.2 mL min?1 and the detection wavelength was 260 nm. The limit of detection for ibuprofen and diphenhydramine citrate was 1.72 and 0.54 μg mL?1 and the limit of quantification was 5.73 and 1.64 μg mL?1, respectively. This method was validated for accuracy, precision and linearity. The method was also found to be stability indicating.  相似文献   

2.
Solid-phase extraction (SPE) and reversed-phase liquid chromatography (RP-LC) have been used for simple, sensitive simultaneous analysis of cyromazine and melamine residues in liquid milk and eggs. The conditions used for SPE and LC were investigated and optimized. A combined cation-exchange–reversed-phase cartridge was used for clean-up, and an ODS (C18) column (150 mm × 4.6 mm i.d., 5-μm particles) with 62:38 (v/v) 5 mm sodium lauryl sulfate (pH 3.4)–acetonitrile as mobile phase was used for RP-LC. Under the optimum conditions the method limit of detection (LOD) for both cyromazine and melamine was 6.2 μg kg?1 for liquid milk samples, and 11.5 μg kg?1 for egg samples. Average recovery of cyromazine and melamine from milk samples was 90.3%, RSD 4.6–5.6%, and 99.6%, RSD 3.2–4.7%, respectively. Average recovery of cyromazine and melamine from egg samples was 85.3%, RSD 1.0–4.7%, and 89.6%, RSD 3.1–5.0%, respectively. The method enables detection of melamine and cyromazine at levels as low as 20.7 μg kg?1 in liquid milk and 38.3 μg kg?1 in egg.  相似文献   

3.
A new method involving matrix solid-phase dispersion (MSPD) extraction and UPLC in conjunction with photodiode array detection was developed for the rapid and simple determination of Sudan dyes in chili powder. Separation of Sudan I, Sudan II, Sudan III, and Sudan IV was achieved within 2 min on the 1.7 μm Acquity UPLC BEH C18 column by using gradient elution with a mobile phase consisting of acetonitrile–water at a flow rate of 0.5 mL min?1. Optimization of MSPD extraction parameters, such as type of solid sorbent and elution solvent were carried out. Optimal conditions selected for MSPD extraction were 0.25 g of sample, 0.5 g of silica gel as solid sorbent, and 7 mL of acetonitrile–methanol (9:1, v/v) as eluting solvent. Limits of detection ranged between 0.25 and 0.30 mg kg?1 depending on the dye involved. All analytes provided average recoveries from spiked (at 1, 1.5, and 2 mg kg?1) chili powder samples ranging from 81 to 106%. The method was applied to the analysis of chili powder samples obtained from different countries.  相似文献   

4.
Hongzhe Tian 《Chromatographia》2011,73(5-6):457-462
A method for determination of chlormequat (CCC) residue in fruits by liquid chromatography?Ctandem mass spectrometry (LC?CMS?CMS) was developed. Residue of CCC was extracted from samples with methanol?Cwater (v/v, 1:1) containing 1.0% acetic acid, cleaned up by strong cationic exchange (SCX) cartridge, and then determined by LC?CMS?CMS. The method showed good linearity over the concentration range 0.002?C5.0 mg kg?1 with correlation coefficient above 0.997. The limit of detection (LOD) and limit of quantitation (LOQ) for CCC were 5 × 10?4 mg kg?1 (S/N = 3) and 0.002 mg kg?1 (S/N = 10), respectively. Recoveries for CCC at three spiked levels (0.025, 0.050, and 0.20 mg kg?1) were in the range 80?C102%. Estimation of measurement uncertainty was calculated for CCC at the level of 0.025 mg kg?1 in fruits. The results demonstrated that the uncertainty of recovery was the main contribution to the combined standard uncertainty. The relative combined standard uncertainties associated with the method ranged from 11 to 13%, depending on the sample matrices.  相似文献   

5.
A rapid, sensitive and specific reversed-phase liquid chromatographic method was developed and validated for the quantification of p-hydroxyphenethyl anisate (HPA), which is one of the main constituents of Notopterygium Radix (underground parts of Notopterygium incisum and N. forbesii), in rat plasma, and study its pharmacokinetics after the intravenous administration of 40 mg kg?1 HPA to rats. The method involves a plasma clear-up step using liquid–liquid extraction by ethyl acetate, followed by RP-LC separation and detection. Separation of HPA was performed on an analytical Diamonsil ODS C18 column equipped with a Dikma ODS C18 EasyGuard column using a mobile phase consisting of MeOH–H2O (75:25, v/v) at a flow-rate of 1.0 mL min?1. The UV detection was performed at a wavelength of 256 nm. The linear calibration curves were obtained in the concentration range of 0.05–5.0 μg mL?1 (r = 0.9992, n = 5) in rat plasma with the lower limit of detection of 0.01 μg mL?1 and the lower limit of quantification of 0.04 μg mL?1, and the extraction recovery of HPA was calculated to be the range of 82.01–86.66%. The intra- and inter-day precisions in terms of % relative standard deviation were lower than 2.33 and 3.99% in rat plasma, respectively, with accuracies ranging from 91.22 to 110.5%. The developed method was suitable for the determination and pharmacokinetic study of HPA in rat plasma.  相似文献   

6.
A sensitive and specific liquid chromatography–tandem mass spectrometry (LC–MS–MS) method was developed and validated for the quantification of poricoic acid A (PAA) in rat plasma. The plasma samples were precipitated by protein precipitation with methanol. Glycyrrhetic acid was used as the IS. Chromatography was performed on a Dionex C18 120 Å (4.6 × 250 mm, 5 μm) column with the mobile phase composed of acetonitrile–water (90:10, v/v) at a flow rate of 0.8 mL min?1. A tandem mass spectrometer equipped with an ESI source was used as the detector and was operated in the negative ion mode. Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 497.4 → 423.3 and m/z 469.2 → 425.1 for PAA and IS, respectively. The calibration curves were linear over the range of 5–5,000 ng mL?1 (r 2 = 0.9966) and the lower limit of quantification (LLOQ) was 5 ng mL?1. In this range, RSDs were <10% for intra-assay and inter-assay precisions. The accuracy expressed by deviation (DEV) was <6%, and the extraction recoveries of QC samples were >78%. The validated method was successfully used to study the pharmacokinetics of PAA in rats after intravenous administration at a dose of 1.0, 2.5 and 5.0 mg kg?1 and oral administration at a dose of 25, 50 and 100 mg kg?1, respectively. The relative bioavailability of PAA in rats following oral administration was achieved.  相似文献   

7.
An extraction method based on matrix solid-phase dispersion was developed to determine carbofuran, pyrimethanil and tetraconazole in banana using gas chromatography–mass spectrometry. The best results were obtained using 2.0 g of banana, 1.0 g of silica as dispersant sorbent and n-hexane:ethyl acetate (1:4, v/v) as eluting solvent. The method was validated using banana samples fortified with pesticides at different concentration levels (0.05–2.0 mg kg?1). Average recoveries (four replicates) ranged from 68 to 111%, with relative standard deviations between 6.6 and 20.5%. Detection and quantification limits for banana ranged from 0.02 to 0.05 and 0.05 to 0.10 mg kg?1, respectively.  相似文献   

8.
A sensitive and reliable reversed-phase liquid chromatography (RP-LC) with ultraviolet (UV) detection has been developed and validated for the quantification of Icariside II in rat plasma and tissues using Fermononetin as the internal standard. Protein precipitation and liquid?Cliquid extraction were utilized for plasma and tissue sample preparation, respectively. The analysis was successfully carried out on an Agilent SB-C18 column (5 ??m, 4.6 × 250 mm) with the implementation of the following conditions: a mobile phase of phosphoric acid solution (0.1%, v/w)?CAcetonitrile (55:45, v/v), a flow rate of 1 mL min?1, a column temperature of 25 °C and a detection wavelength of 270 nm. Good linear relationships of calibration curves were obtained (r 2 > 0.9906) over the investigated concentration range with plasma and tissue samples. The lower limit of quantification (LLOQ) and the limit of detection (LOD) were 0.1 and 0.02 ??g g?1, respectively (for plasma sample, they were 0.05 and 0.1 ??g mL?1, respectively). The developed method which was embodied with good precision, accuracy, recovery and stability was corroborated to satisfy the requirements for biomedical sample analysis. This method has been successfully applied to tissue distribution study of Icariside II in rats after a single intravenous dose at 12.5 mg kg?1. Results suggested that Icariside II was distributed to rat tissues rapidly with greater initial concentrations in kidney, lung and liver. Moderate initial distributions were obtained in rat muscle, heart, bone, spleen and plasma. Low amount of Icariside II was detected in testes, and no Icariside II could be detected in the brain.  相似文献   

9.
A simple, rapid and sensitive high-performance liquid chromatography LC (HPLC) method of determining the concentration of the novel betulinic acid derivative DRF-4012 (5??-chloro-2,3-didehydroindolo[2??,3??:2,3]betulinic acid) in rat plasma for pharmacokinetic and toxicokinetic purposes has been developed and validated. A simple and fast protein precipitation was performed, and then an extraction using an ethyl acetate:methanol (75:25 v/v) mixture was used to extract DRF-4012 and an internal standard (IS, DRF-4015) from rat plasma. Chromatographic separation was achieved using a Zorbax Eclipse XDB-C8 reversed-phase column with UV detection at 235 nm. The isocratic mobile phase, phosphate buffer (water adjusted to pH 3 with 20% o-phosphoric acid) and acetonitrile (15:85, v/v), was run at a flow rate of 1.2 mL min?1. The assay was linear (r 2 > 0.99) over the concentration range 0.040?C75.0 ??g mL?1, and presented limits of detection and quantification of 0.020 and 0.040 ??g mL?1, respectively, in rat plasma. The absolute recovery of both the analyte and the IS was >85% from rat plasma. The intraday accuracy ranged from 99.25 to 102.67% with a precision of 2.62?C4.48%, and the interday accuracy ranged from 98.48 to 104.56% with a precision of 3.87?C5.68%. This developed and validated method was successfully used to determine the DRF-4012 concentration in rat plasma for a pharmacokinetic and toxicokinetic study after the intravenous administration of a 1 mg mL?1 DRF-4012 nanoparticle formulation at doses of 2?C10 mg kg?1 in Wistar rats.  相似文献   

10.
A reversed-phase liquid chromatography coupled to tandem mass spectrometry (LC?CMS?CMS) method was developed and validated for the determination of fulvestrant in rat plasma. Sample preparation involved a liquid-liquid extraction using 1.0 mL of n-hexane?Cisopropanol (90:10, v/v) to extract the analyte from 0.1 mL of rat plasma. The analytes were separated on a phenyl-based column using the mobile phase consisting of methanol/water containing 5 mM ammonium acetate at the flow rate of 0.3 mL min?1. The analytes were monitored by tandem mass spectrometry under electrospray negative ionization mode. Linear calibration curves were generated over the fulvestrant concentration ranges of 0.05?C10.0 ng mL?1 in rat plasma. The accuracy and within- and between-day precisions were within the generally accepted criteria for bioanalytical methods (<15%). This developed and validated assay method was successfully employed to characterize the plasma concentration-time profile of fulvestrant after its intramuscular administration in rats at a dose of 10 mg kg?1.  相似文献   

11.
A reversed-phase liquid chromatographic method was established for the simultaneous determination of imperatorin and isoimperatorin in eleven kinds of traditional Chinese medicinal preparations (TCMPs) containing Radix Angelicae dahuricae (Chinese herbal name: Baizhi). Imperatorin and isoimperatorin were successfully separated on an Ultimate XB-C18 column (150 mm × 4.6 mm i.d., 5 μm). The mobile phase was a mixture of acetonitrile and 50 mmol L?1 sodium acetate (pH 3.5) buffer (45:55, v/v), employing isocratic elution at a flow rate of 1.0 mL min?1. Detection was accomplished at 302 nm. Regression equations revealed good linear relationship between the peak areas of the constituents and their concentrations (correlation coefficients: 0.9995 for imperatorin, 0.9991 for isoimperatorin). The recoveries were between 97.38% and 103.78%. The proposed method has been successfully applied to the simultaneous determination of imperatorin and isoimperatorin in eleven kinds of TCMPs containing Baizhi.  相似文献   

12.
A simple and sensitive liquid chromatographic assay with fluorescence detection assay was developed for the determination of zearalenone levels in rat serum. The assay utilized a single liquid–liquid extraction with t-butyl methyl ether and isocratic elution using a mobile phase consisting of acetonitrile and 0.1% triethylamine in distilled water (pH = 6) (50:50, v/v). Linearity was observed over a concentration range from 10 to 1,000 ng mL?1 (r = 0.9995), with the limit of quantification at 10 ng mL?1 with 100 μL of rat serum. The validated assay was applied to a pharmacokinetic study in rats.  相似文献   

13.
A new stability-indicating reversed-phase LC method has been developed and validated for the assay and identification of betamethasone dipropionate and its related compounds in a dermatological pharmaceutical drug product, namely Diprolene Ointment. Separation of all the peaks of interest was achieved on a Symmetry Shield RP18 (100 mm × 4.6 mm, 3.5 µm) column using a gradient elution at a flow rate of 1.5 mL min?1 with mobile phase A (10 mM monobasic sodium phosphate at pH 2.5) and mobile phase B (acetonitrile) and UV detection at 250 nm. The limit of detection (LOD) and limit of quantitation (LOQ) of this method was 0.00004  and 0.0001 mg mL?1, respectively. The method was successfully validated in accordance with ICH guidelines and was accurate, linear, precise, reproducible, specific, and robust. A simple, reproducible and accurate single step sample extraction procedure using tetrahydrofuran, water, and methanol (40:30:30, v/v/v) was developed to extract betamethasone dipropionate and its related compounds from the ointment. The sample extraction procedure and the LC conditions presented in this report can be used for routine analysis of Diprolene Ointment in quality control laboratories. This method may also be applied to other dermatological pharmaceutical drug products “as-is” or with minor modification.  相似文献   

14.
A simple and sensitive liquid chromatographic method was developed for quantification of cefteram in human plasma. Amoxicillin was used as an internal standard. The present method used protein precipitation for extraction of cefteram from human plasma. Separation was carried out on a reversed-phase C18 column. The column effluent was monitored by UV detection at 262 nm. The mobile phase was a mixture of methanol and water containing 0.3% v/v triethylamine and 0.6% v/v glacial acetic acid (35:65:0.3:0.6 v/v) at a flow rate of 0.30 mL min?1. The column temperature was 20 °C. This method was linear over the range of 47.5–4,750.0 ng mL?1 with determination coefficient greater than 0.99. The mean extraction recovery of cefteram and IS was ≥76.82 and ≥76.49%, respectively, and the method was found to be precise, accurate, and specific during the study. The method was successfully applied for a pharmacokinetic study of cefteram in human.  相似文献   

15.
Pesticides are widely used in rice cultivation, often resulting in detection of their residues in rice grains. So far, no analytical method has been available for the simultaneous determination of most rice pesticides in rice grains. This paper reports the development and validation of such a method for the determination of eight rice pesticides (penoxsulam tricyclazole, propanil, azoxystrobin, molinate, profoxydim, cyhalofop-butyl, deltamethrin) and 3,4-dichloroaniline, the main metabolite of propanil. Pesticide extraction and clean-up was performed by an optimized matrix solid-phase dispersion (MSPD) protocol on neutral alumina (5 g) using acetonitrile as the elution solvent. Samples were analyzed in a high-performance liquid chromatography–diode array detection (HPLC-DAD) system. Pesticide separation was achieved with a mobile phase of acetonitrile/water in a linear elution gradient from 30:70% (v/v) to 100:0% (v/v) in 14 min at a flow rate of 0.8 mL min?1. Method validation was performed by means of linearity, intra-day accuracy, inter-day precision and sensitivity. Linear regression coefficients (R 2) were always above 0.9948. Limits of detection (LOD) and quantification (LOQ) varied from 0.002 to 0.200 mg kg?1 and 0.006 to 0.600 mg kg?1, respectively. Recoveries were investigated at three fortification levels and were found to be acceptable (74–127%) with relative standard deviations (RSD) below 12%. Application of the method for the analysis of five commercial rice grain samples showed that the pesticide levels were below the LOD. Overall, the method developed is suitable for the determination of residues of most rice pesticides in rice grains at levels below the established MRLs.  相似文献   

16.
ent-11α-Hydroxy-15-oxo-kaur-16-en-19-oic acid (5F), a diterpenoid isolated from the Chinese herb Pteris semipinnata L, has been suggested to show antitumor properties. A simple and sensitive LC method was developed for the determination of 5F in rabbit plasma. The method involved liquid–liquid extraction using ethyl acetate under acidic conditions using naproxen as an internal standard. Separations were performed on a reversed-phase column with a mixture of 1% (v/v) glacial acetic acid and methanol (45:55, v/v) as mobile phase and UV detection was utilized at 242 nm. The calibration plot was linear in the range 0.20–10.0 μg mL?1 (correlation coefficients r 2  > 0.998). The detection limit was 0.20 μg mL?1, mean extraction recovery was above 82%, intra-day precision of the method was less than 6.4%, and inter-day precision was better than 8.7%, respectively. The validated assay was found to be suitable for the pharmacokinetic study of 5F in rabbits.  相似文献   

17.
We present a simple and reliable method for simultaneous determination of voriconazole and its main metabolite resulting from N-oxidation (UK-121,265), in human plasma. The work-up procedure used acetonitrile and potassium salts to precipitate plasma proteins. No internal standard was used. The chromatographic system used a LiChroCART® 250-4 cartridge packed with LiChrospher® 100 RP-8 (diameter particules, 5 μm). The UV monochromatic detector was set on 260 nm. The mobile phase consisted of a 60/40 (v/v) mixture of acetonitrile and water. The flow rate was 1 mL min?1. The retention times for voriconazole and its metabolite were 8.98 and 4.02 min respectively, and total run time was 12 min. The linearity of the method was investigated from 0.31 to 10.0 mg L?1; the lowest limit of quantification was 0.30 mg L?1. Precision ranged from 2.41% to 6.32% for voriconazole and 0.80% to 11.6% for the N-oxide voriconazole metabolite. Accuracy was between 93.0% and 101% for voriconazole and 90.0% and 101% for the N-oxide voriconazole metabolite. This rapid and accurate method could be interesting to investigate metabolite/voriconazole ratio with respect to CYP2C19 genetic status and CYP3A4 activity changes.  相似文献   

18.
A rapid method was developed for the determination of pentachloronitrobenzene (PCNB) and its metabolites pentachloroaniline, pentachlorothioanisole residues in ginseng. Extraction and clean-up were carried out in a single step and analysis was accomplished by gas chromatography–mass spectrometry with multiple reaction monitoring. The main parameters affecting extraction yield and selectivity, such as type and amount of dispersant material, clean-up co-sorbent and extraction solvent were evaluated. The best results were obtained using 1 g ginseng, 2 g florisil as dispersant sorbent, 0.5 g neutral alumina as clean-up co-sorbent, and subsequent extraction with 10 mL acetone–n-hexane (5:5, v/v) with assisted sonication and repeated with another 5 mL of the same solvent mixture. The method was validated by analysis of ginseng samples fortified at different concentration levels (0.01–0.10 mg kg?1). Average recoveries (n = 5) ranged from 85 to 95% with relative standard deviation between 2.5 and 11.2%. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The detection limits ranged from 0.2 to 0.9 µg kg?1 in ginseng. The method was applied to the analysis of PCNB and its metabolite residues in commercial ginseng samples.  相似文献   

19.
A robust and sensitive method was developed for the simultaneous analysis of metribuzin and quizalofop-p-ethyl residues in potato and soil, based on solid-phase extraction (SPE) coupled to capillary gas chromatography with electron capture detector (GC-ECD). Residues of two herbicides were extracted from potato and soil with acetone and methanol–water, followed by SPE to remove coextractives, before analysis by GC-ECD. SPE procedures were performed on Florisil cartridges (500 mg, 3 mL), the analytes from potato and soil matrix were eluted with petroleum ether-acetic ether (9:1 v/v, 5 mL) and petroleum ether-acetic ether (8:2 v/v, 2 mL), respectively. Limits of quantification of the method were 0.01 mg kg?1, and the mean recoveries ranged from 72.9 to 109.5% with relative standard deviation ranging from 0.7 to 9.2% at the three spike levels (0.01, 0.1, and 0.5 mg kg?1). The proposed method was successfully applied to the analysis of metribuzin and quizalofop-p-ethyl residues in potato and soil samples from an experimental field. Direct confirmation of the analytes in real samples was achieved by gas chromatography-mass spectrometry (GC–MS).  相似文献   

20.
A novel and simple liquid chromatographic (LC) method was developed for quantification of a new anticancer compound, chloride 3-methyl-9-(2-oxa-2λ5-2H-1,3,2-oxazaphosphorine-2-cyclohexyl)-3,6,9-triazaspiro [5.5] undecane (SLXM-2) in rat plasma. The present method used protein precipitation for extraction of SLXM-2 from rat plasma. Separation was carried out on a reversed-phase C18 column (150 mm × 4.6 mm i.d., 5 μm). The mobile phases consisted of acetonitrile and 2 mM sodium dodecyl sulfate (SDS) (24:76, v/v). The flow rate was 1.0 mL min?1. A diode-array detector (DAD) was used and the column effluent was monitored at 192 nm. Regression equations revealed good linear relationship between the peak area and the concentration. The correlation coefficient was 0.9996. The relative standard deviations (RSD) of the precision and accuracy were <9.0% (intra-day) and <6.1% (inter-day), respectively. The recovery and stability were found satisfactory during the study. The method was successfully applied for the pharmacokinetic study of SLXM-2 in rats. After a single dose (400 mg kg?1) of SLXM-2 was given to rats by intravenous injection, the half-life of SLXM-2 was 0.304 h, the area under the plasma concentration–time curve was 673.1 μg h mL?1 and the maximal plasma concentration was 1534.9 ± 185.8 μg mL?1.  相似文献   

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