共查询到20条相似文献,搜索用时 15 毫秒
1.
Derya Aşangil İbrahim Hüdai Taşdemir Esma Kılıç 《Journal of Pharmaceutical Analysis》2012,2(3):193-199
Anodic behavior of aripiprazole (ARP) was studied using electrochemical methods. Charge transfer, diffusion and surface coverage coefficients of adsorbed molecules and the number of electrons transferred in electrode mechanisms were calculated for quasi-reversible and adsorption-controlled electrochemical oxidation of ARP at 1.15 V versus Ag/AgCl at pH 4.0 in Britton–Robinson buffer (BR) on glassy carbon electrode. Voltammetric methods for direct determination of ARP in pharmaceutical dosage forms and biological samples were developed. Linearity range is found as from 11.4 μM (5.11 mg/L) to 157 μM (70.41 mg/L) without stripping mode and it is found as from 0.221 μM (0.10 mg/L) to 13.6 μM (6.10 mg/L) with stripping mode. Limit of detection (LOD) was found to be 0.11 μM (0.05 mg/L) in stripping voltammetry. Methods were successfully applied to assay the drug in tablets, human serum and human urine with good recoveries between 95.0% and 104.6% with relative standard deviation less than 10%. 相似文献
2.
Yan Li Xiao-Rong Liu Xiao-Hui Ning Can-Can Huang Jian-Bin Zheng Jun-Cai Zhang 《Journal of Pharmaceutical Analysis》2011,1(4):258-263
An electrochemical sensor incorporating a signal enhancement for the determination of lead (II) ions (Pb2+) was designed on the basis of the thrombin-binding aptamer (TBA) as a molecular recognition element and ionic liquid supported cerium oxide (CeO2) nanoparticles–carbon nanotubes composite modification. The composite comprises nanoparticles CeO2, multi-wall carbon nanotubes (MWNTs) and hydrophobic room temperature ionic liquid (RTIL) 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF4). The electrochemical sensors were fabricated by immersing the CeO2–MWNTs–EMIMBF4 modified glassy carbon electrode (GCE) into the solution of TBA probe. In the presence of Pb2+, the TBA probe could form stable G-quartet structure by the specific binding interactions between Pb2+ and TBA. The TBA-bound Pb2+ can be electrochemically reduced, which provides a readout signal for quantitative detection of Pb2+. The reduction peak current is linearly related to the concentration of Pb2+ from 1.0×10–8 M to 1.0×10–5 M with a detection limit of 5×10–9 M. This work demonstrates that the CeO2–MWNTs–EMIMBF4 nanocomposite modified GCE provides a promising platform for immobilizing the TBA probe and enhancing the sensitivity of the DNA-based sensors. 相似文献
3.
《Journal of Pharmaceutical Analysis》2014,4(5):325-330
A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were well separated on a C18 column and detected with high sensitivity. A mobile phase containing acetonitrile and 10 mM Na2HPO4–H3PO4 (pH 5.0) (50:50, v/v) was used. Good linearity was obtained in the range of 0.208–41.6, 0.197–39.4, and 0.227–114 μM for curcumin, demethoxycurcumin and bisdemethoxycurcumin respectively. The limit of detection reached up to 10−8 M, which was lower than that by UV detection. The relative standard deviations (RSDs) ranged from 1.06% to 1.88% for intra-day precision and from 4.30% to 5.79% for inter-day precision, respectively. The proposed method has been applied in real herb sample and recoveries ranging from 86.3% to 111% were obtained. 相似文献
4.
A novel method for the simultaneous high-performance liquid chromatographic determination of nortriptyline hydrochloride and fluphenazine hydrochloride was developed and validated. Fluvastatin sodium was used as internal standard. The determination was performed on a Hypersil Gold C8 column (250 mm × 4.6 mm i.d., 5 μm particle size) at 25 °C; the mobile phase, consisting of a mixture of formic acid (0.1 M, pH 2.16)-methanol (33:67, v/v), was delivered at a flow rate of 1.1 mL/min and detector wavelength at 251 nm. The retention time of nortriptyline, fluphenazine and fluvastatin was found to be 5.11, 8.05 and 11.38 min, respectively. Linearity ranges were 5.0–1350.0 and 10.0–1350.0 μg/mL with limit of detection values of 0.72 and 0.31 μg/mL, for nortriptyline and fluphenazine, respectively. Results of assay and recovery studies were statistically evaluated for its accuracy and precision. Correlation coefficients (r2) of the regression equations were greater than 0.999 in all cases. According to the validation results, the proposed method was found to be specific, accurate, precise and could be applied to the simultaneous quantitative analysis of nortriptyline and fluphenazine. 相似文献
5.
M. Mathrusri Annapurna S.V.S. Goutam S. Anusha L. Srinivas 《Journal of Pharmaceutical Analysis》2012,2(6):466-469
An isocratic RP-HPLC method was developed for the determination of Cefditoren pivoxil in pharmaceutical formulations using a C-18 column with water–acetonitrile (50:50, v/v) as mobile phase and flow rate 1.2 mL/min (UV detection at 218 nm). Linearity was observed in the concentration range 1.0–250 μg/mL (R2=0.999) with regression equation y=24194x+10749. The forced degradation studies were performed by using HCl, NaOH, and H2O2, and thermal and UV radiation. Cefditoren pivoxil is more sensitive towards oxidation and alkaline conditions and resistant towards acidic and photolytic degradations. The method was validated as per ICH guidelines. 相似文献
6.
Vamsi Krishna Marothu Rajendra N. Dash Saritha Vemula Shravani Donkena Ramesh Devi Madhavi Gorrepati 《Journal of Pharmaceutical Analysis》2012,2(6):431-436
An isocratic stability indicating RP-HPLC–UV method is presented for the determination of metaxalone (MET) in the presence of its degradation products. The method uses Dr. Maisch C18 column (250 mm×4.6 mm, 5 μm) with mobile phase consisting of acetonitrile–potassium dihydrogen orthophosphate buffer with 4 mL of 0.4% triethyl amine (pH 3.0; 10 mM) (58:42, v/v) at a flow rate of 1.0 mL/min. pH of the buffer was adjusted with o-phosphoric acid. UV detection was performed at 225 nm. The method was validated for specificity, linearity, precision, accuracy, limit of detection, limit of quantification and robustness. The calibration plot was linear over the concentration range of 1–100 μg/mL having a correlation coefficient (r2) of 0.999. Limits of detection and quantification were 0.3 and 1 μg/mL, respectively. Intra-day and inter-day precision (% RSD) was 0.65 and 0.79 respectively. The proposed method was used to investigate the degradation kinetics of MET under different stress conditions employed. Degradation of MET followed a pseudo-first-order kinetics, and rate constant (K), time left for 50% potency (t1/2), and time left for 90% potency (t90) were calculated. 相似文献
7.
Vasu Babu Ravi Jaswanth Kumar Inamadugu Nageswara Rao Pilli Vudagandla Sreenivasulu Venkateswarlu Ponneri 《Journal of Pharmaceutical Analysis》2012,2(5):319-326
A rapid and sensitive liquid chromatography–tandem mass spectrometric (LC–MS/MS) assay method has been developed and fully validated for the simultaneous quantification of telmisartan and amlodipine in human plasma. Carbamazepine was used as an internal standard. Analytes and the internal standard were extracted from human plasma by solid-phase extraction technique using Waters Oasis® HLB 1 cm3 (30 mg) extraction cartridge. The reconstituted samples were chromatographed on a Hypurity advance C18 column (50 mm×4.6 mm, 5 μm) using a mixture of acetonitrile–5 mM ammonium acetate buffer (pH-4.0) (50:50, v/v) as the mobile phase at a flow rate of 0.8 mL/min. The calibration curve obtained was linear (r≥0.99) over the concentration range of 2.01–400.06 ng/mL for telmisartan and 0.05–10.01 ng/mL for amlodipine. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 400 human plasma samples per day. The proposed method was found to be applicable to clinical studies. 相似文献
8.
A novel flow injection chemiluminescence (CL) method for the determination of loxoprofen and naproxen was proposed based on the CL system of KMnO4, and Na2SO3 in acid media. The CL intensity of KMnO4-Na2SO3 was greatly enhaneed in the presence of loxoprofen and naproxen. The mechanism of the CL reaction was studied by the kinetic proecss and UV-vis absorption and the conditions were optimized. Under optimized conditions, the CL intensity was linear with loxoprofen and naproxen concentration in the range of 7.0 × 10?8 – 1.0 × 10?5 g/mL and 2.0 × 10?7 – 4.0 × 10?6 g/mL with the detection limit of 2.0 × 10?8 g/mL and 3.0 × 10?8 g/mL (S/N = 3), respectively. Thc relative standard deviations were 2.39% and 1.37% for 5.0 × 10?7 g/mL naproxen and 5.0 × 10?7 g/mL loxoprofen (n = 10), respectively. The proposed method was satisfactorily applied to thc determination of loxoprofen and naproxen in pharmaceutical preparations. 相似文献
9.
Zi-You Cai Yong-Chong Li Li-Hua Li Zuan-Guang Chen 《Journal of Pharmaceutical Analysis》2012,2(5):356-360
A new method for the determination of arecoline in Semen Arecae decoction pieces by microchip capillary electrophoresis with contactless conductivity detection (MCE-CCD) was proposed. The effects of various electrophoretic operating parameters on the analysis of arecoline were studied. Under the optimal conditions, arecoline was rapidly separated and detected in 1 min with good linearity over the concentration range of 20–1500 μM (r2=0.9991) and the detection limit of 5 μM (S/N=3). The method was used for the analysis of arecoline satisfactorily with a recovery of 96.8–104%. 相似文献
10.
Ashraf M. Mahmoud Hanaa M. Abdel-Wadood Niveen A. Mohamed 《Journal of Pharmaceutical Analysis》2012,2(5):334-341
A simple and sensitive kinetic spectrophotometric method has been developed and validated for determination of amlodipine besylate (AML). The method was based on the condensation reaction of AML with 7-chloro-4-nitro-2,1,3-benzoxadiazole in an alkaline buffer (pH 8.6) producing a highly colored product. The color development was monitored spectrophometrically at the maximum absorption λmax 470 nm. The factors affecting the reaction were studied and the conditions were optimized. The stoichiometry of the reaction was determined, and the reaction pathway was postulated. Moreover, both the activation energy and the specific rate constant (at 70 °C) of the reaction were found to be 6.74 kcal mole?1 and 3.58 s?1, respectively. The initial rate and fixed time methods were utilized for constructing the calibration graphs for the determination of AML concentration. Under the optimum reaction conditions, the limits of detection and quantification were 0.35 and 1.05 μg/mL, respectively. The precision of the method was satisfactory; the relative standard deviations were 0.85–1.76%. The proposed method was successfully applied to the analysis of AML in its pure form and tablets with good accuracy; the recovery percentages ranged from 99.55±1.69% to 100.65±1.48%. The results were compared with that of the reported method. 相似文献
11.
Patrícia Severino Heloisa Silva Eliana B. Souto Maria Helena A. Santana Teresa Cristina T. Dalla Costa 《Journal of Pharmaceutical Analysis》2012,2(1):29-34
Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV). An automated system using on-line solid extraction and High Performance Liquid Chromatography (HPLC) with ultraviolet (UV) detection was developed and validated for pharmacokinetic analysis of didanosine in dog plasma. Modifications were introduced on a previous methodology for simultaneous analysis of antiretroviral drugs in human plasma. Extraction was carried out on C18 cartridges, with high extraction yield as stationary phase, whereas mobile phase consisted of a mixture of 0.02 M potassium phosphate buffer, acetonitrile (KH2PO4: acetonitrile: 96:4, v/v) and 0.5% (w/v) of heptane sulphonic acid. The pH was adjusted to 6.5 with triethylamine. All samples and standard solutions were chromatographed at 28 °C. For an isocratic run, the flux was 1.0 mL/min, detection was at 250 nm and injected volume was 20 μL. The method was selective and linear for concentrations between 50 and 5000 ng/mL. Drug stability data ranged from 96% to 98%, and limit of quantification was 25 ng/mL. Extraction yield was up to 95%. Drug stability in dog plasma was kept frozen at ?20 °C for one month after three freeze–thaw cycles, and for 24 h after processing in the auto sampler. Assay was successfully applied to measure didanosine concentrations in plasma dogs. 相似文献
12.
Ravi Kumar Konda Babu Rao Chandu B.R. Challa Chandrasekhar B. Kothapalli 《Journal of Pharmaceutical Analysis》2012,2(5):342-349
The most suitable bio-analytical method based on liquid–liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm×50 mm, 3.5 μm) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The total run time was 3.0 min. The proposed method has been validated with the linear range of 5–12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3%–2.9% and 1.6%–2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-13C3 mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition. 相似文献
13.
M. Mathrusri Annapurna Chitaranjan Mohapatro A. Narendra 《Journal of Pharmaceutical Analysis》2012,2(4):298-305
A stability-indicating high-performance liquid chromatographic method was developed and validated for the determination of Letrozole in tablet dosage forms. Reversed-phase chromatography was performed on Shimadzu Model LC-Class-Vp with Lichrocart/Lichrosphere 100 C-18 (250 mm×4.6 mm, 5 μm particle size) column with methanol: tetra butyl ammonium hydrogen sulfate (80:20V/V) as mobile phase at a flow rate of 1 mL/min with UV detection at 240 nm. Linearity was observed in the concentration range of 0.5–150 μg/mL (R2=0.9998) with regression equation y=102582x+43185. The limit of quantitation (LOQ) and limit of detection (LOD) were found to be 0.043 and 0.012 μg/mL respectively. The forced degradation studies were performed by using HCl, NaOH, H2O2, thermal and UV radiation. Letrozole is more sensitive towards alkaline conditions and very much resistant towards acidic, oxidative and photolytic degradations. The method was validated as per ICH guidelines. The RSD for intra-day (0.78–0.97) and inter-day (0.86–0.96) precision were found to be lesser than 1%. The percentage recovery was in good agreement with the labeled amount in the pharmaceutical formulations and the method is simple, specific, precise and accurate for the determination of Letrozole in pharmaceutical formulations. 相似文献
14.
A sensitive electroanalytical method for quantification of pheniramine in pharmaceutical formulation has been investigated on the basis of the enhanced electrochemical response at glassy carbon electrode modified with multi-walled carbon nanotubes in the presence of sodium lauryl sulfate. The experimental results suggest that the pheniramine in anionic surfactant solution exhibits electrocatalytic effect resulting in a marked enhancement of the peak current response. Peak current response is linearly dependent on the concentration of pheniramine in the range 200–1500 μg/mL with correlation coefficient 0.9987. The limit of detection is 58.31 μg/mL. The modified electrode shows good sensitivity and repeatability. 相似文献
15.
Nitin Dubey Nidhi Dubey Mayank Mandhanya Dinesh Kumar Jain 《Journal of Pharmaceutical Analysis》2012,2(6):478-483
Prevention of cross contamination with active pharmaceutical ingredients is crucial and requires special attention in pharmaceutical industries. Current method validation describes the determination of Nabumetone (NAB) residue on a stainless steel surface using swab sampling with a sensitive HPLC-DAD analysis. The acceptance limit was decided as 2 μg swab per 100 cm2. Cotton swabs impregnated with extraction solution were used to determine residual drug content. Recoveries were 90.88%, 91.42%, and 92. 21% with RSD ranging from 2.2% to 3.88% at three concentration levels. Residual concentration was found to be linear in the range of 0.1–4.56 μg/mL, when estimated using a Phenomenex Luna C18 (25 cm×5 μm×4.6 mm i.d.) column at 1.0 mL/min flow rate and 230 nm. The mobile phase consisted of a mixture of methanol:acetonitrile:water (55:30:15, v/v/v). The LOD and LOQ for NAB were found to be 0.05 and 0.16 μg/mL, respectively. The validated method was found to be simple, selective and sensitive for demonstration of cleaning validation of NAB residues on a stainless steel surface. 相似文献
16.
Ze-Yun Li Qing Li Jiang Lü Jun-Hong Ling Xi-Hua Yu Xiao-Hui Chen Kai-Shun Bi 《Journal of Pharmaceutical Analysis》2011,1(1):8-12
A simple, rapid and sensitive liquid chromatography-mass spectrometry (LC-MS) method was developed for the determination of salidroside in rat plasma and study of its pharmacokinetics after oral administration of suspension of Erzhi Wan and Fructus Ligustri lucidi into Wistar rats. Plasma sample of 200 μL was extracted with acetic ether-isopropanol (2:1) and the extraction was performed on a Kromasil C18 column (150 mm × 4. 6 mm, 5 μm) with the mobile phase of methanol-water (41:59, v/v) within a run time of 6.0 min. The analyte was monitored with positive electrospray ionization (ESI) by selected ion monitoring (SIM) mode. The target ions were m/z 323.05 for salidroside and m/z 411.05 for internal Standard (IS) geniposide. A good linear relationship was obtained over the range of 5.0–500.0 ng/mL and the lower limit of quantification was 5.0 ng/mL. The validated method was successfully applied to the pharmacokinetic study of salidroside in rat plasma after oral administration of suspension of Erzhi Wan and Fructus Ligustri lucidi. 相似文献
17.
《Journal of Pharmaceutical Analysis》2014,4(5):331-338
In this work, the nickel–aluminum layered double hydroxide (Ni–Al LDH) with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbent for the selective separation and pre-concentration of mefenamic acid prior to quantification by UV detection at λmax=286 nm. Extraction procedure is based on the adsorption of mefenamate anions on the Ni–Al(NO3−) LDH and/or their exchange with LDH interlayer NO3− anions. The effects of several parameters such as cations and interlayer anions type in LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent and co-existing ions on the extraction were investigated and optimized. Under the optimum conditions, the calibration graph was linear within the range of 2–1000 µg/L with a correlation coefficient of 0.9995. The limit of detection and relative standard deviation were 0.6 µg/L and 0.84% (30 µg/L, n=6), respectively. The presented method was successfully applied to determine of mefenamic acid in human serum and pharmaceutical wastewater samples. 相似文献
18.
《Journal of Pharmaceutical Analysis》2014,4(2):144-152
A validated ultra-performance liquid chromatography mass spectrometric method (UPLC–MS/MS) was used for the simultaneous quantitation of candesartan (CN) and hydrochlorothiazide (HCT) in human plasma. The analysis was performed on UPLC–MS/MS system using turbo ion spray interface. Negative ions were measured in multiple reaction monitoring (MRM) mode. The analytes were extracted using a liquid–liquid extraction (LLE) method by using 0.1 mL of plasma volume. The lower limit of quantitation for CN and HCT was 1.00 ng/mL whereas the upper limit of quantitation was 499.15 ng/mL and 601.61 ng/mL for CN and HCT respectively. CN d4 and HCT-13Cd2 were used as the internal standards for CN and HCT respectively. The chromatography was achieved within 2.0 min run time using a C18 Phenomenex, Gemini NX (100 mm×4.6 mm, 5 µm) column with organic mixture:buffer solution (80:20, v/v) at a flow rate of 0.800 mL/min. The method has been successfully applied to establish the bioequivalence of candesartan cilexetil (CNC) and HCT immediate release tablets with reference product in human subjects. 相似文献
19.
A simple, precise, and rapid high-performance liquid chromatographic method was developed and validated for the simultaneous determination of vitexin-2″-O-glucoside, vitexin-2″-O-rhamnoside, rutin, vitexin, and hyperoside. The HPLC separation was performed using a Shim-pack VP-ODS C18 column (250 mm×4.6 mm i.d., 5 μm) with the isocratic mobile phase consisting of tetrahydrofuran/ acetonitrile/0.05% phosphoric acid solution (20:3:77, v/v/v), and the flow rate was set at 1.0 mL/min. UV detection was carried out at a wavelength of 360 nm and the whole analysis took 25 min. The method was linear in the range of 4.12–206.00 μg/mL for vitexin-2″-O-glucoside, 4.05–202.50 μg/mL for vitexin-2″-O-rhamnoside, 1.64–82.00 μg/mL for rutin, 1.74–87.00 μg/mL for vitexin, and 1.41–70.60 μg/mL for hyperoside with the correlation coefficient for each analyte more than 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.6 and 2 ng for vitexin-2″-O-glucoside, 0.6 and 2 ng for vitexin-2″-O-rhamnoside, 0.3 and 1 ng for rutin, 1 and 3 ng for vitexin, and 0.5 and 2 ng for hyperoside, respectively. Intra- and inter-day precision and accuracy (RSD) were less than 3%. The developed HPLC method was successfully applied to the analysis of five flavonoids in hawthorn leaves, hawthorn fruits, and the preparations containing hawthorn leaves or fruits. 相似文献
20.
N.V.V.S.S. Raman A.V.S.S. Prasad K. Ratnakar Reddy K. Ramakrishna 《Journal of Pharmaceutical Analysis》2012,2(4):314-318
Two highly sensitive methods for the determination of genotoxic alkyl methane sulfonates (AMSs) and alkyl paratoluene sulfonates (APTSs) in lamivudine using hyphenated techniques have been presented. AMSs were determined by GC–MS method using GSBP-INOWAX (30 m×0.25 mm×0.25 μm) column. Temperature program was set by maintaining at 100 °C initially for 3 min, then rised to 220 °C at the rate of 15 °C/min and maintained at 220 °C for 16 min. N,N-dimethyl formamide was used as diluent. APTSs were determined by LC-MS using Zorbax, Rx C8, 250 mm×4.6 mm, 5 μm column as stationary phase. 0.01 M ammonium acetate is used as buffer. The mixture of buffer and methanol in 75:25 (v/v) ratio was used as mobile phase A and mixture of buffer and methanol in 5:95 (v/v) ratio was used as mobile phase B. The gradient program (T/%B) was set as 0/28, 16/50, 17/100, 23/100, 27/28 and 40/28. Both the methods were validated as per International Conference on Harmonization guidelines. Limit of quantitation was found 1.5 μg/mL for AMSs and was in the range of 1.0–1.5 μg/mL for APTSs. 相似文献