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1.
A simple and sensitive method has been developed and validated for the determination of aliskiren (ALS) in its dosage forms
and spiked plasma. The method was based on the reaction of the drug with dansyl chloride in the presence of bicarbonate solution
of pH 10.5 to give a highly fluorescent derivative which was measured at 501 nm with excitition at 378 nm in dichloromethane.
Different experimental parameters affecting the development of the method and stability were carefully studied and optimized.
The calibration curves were linear over the concentration ranges of 100–700 and 50–150 ng/mL for standard solution and plasma,
respectively. The limits of detection were 27.52 ng/mL in standard solution, 4.91 ng/mL in plasma. The developed method was
successfully applied to the analysis the drug in the commercial tablets and spiked plasma samples. The mean recovery of ALS
from tablets and plasma was 100.10 and 97.81%, respectively. A proposal of the reaction pathway was presented. 相似文献
2.
Bivash Mandal Pavan Balabathula Nivesh Mittal George C. Wood Himanshu Bhattacharjee 《Journal of fluorescence》2012,22(6):1425-1429
A rapid and sensitive spectrofluorimetric method was developed and validated for the determination of erlotinib (ETB), a potent anticancer drug, in spiked human plasma without any derivatization. The described method was validated and the analytical parameters of linearity, accuracy, precision (intra- and inter-day), limit of detection (LOD), and limit of quantification (LOQ) were evaluated. The relation between the fluorescence intensity and concentration was found to be linear (r2 0.9998) over the range 125 to 1000?ng/mL with the detection limit of 15?ng/mL. A simple liquid-liquid extraction method was followed in order to extract the drug from spiked plasma. The mean absolute recoveries of ETB were 85.59?% (±0.57), 86.91?% (±1.77) and 89.31?% (±3.01) at spiked plasma ETB concentration of 5000, 3750 and 2500?ng/mL, respectively. The spectrofluorimetric method presented here is a rapid, simple, specific, and reproducible method and can be used to characterize the plasma pharmacokinetics of ETB. 相似文献
3.
Simple, accurate and sensitive spectrofluorimetric method has been proposed for the determination of three cephalosporins,
namely; cefixime (cefi), cephalexine (ceph), cefotaxime sodium (cefo) in pharmaceutical formulations. The method is based
on a reaction between cephalosporins with 1, 2-naphthoquinone-4-sulfonic (NQS) in alkaline medium, at pH values of 12.0 for
cefi and 13.0 for ceph and cefo to give highly fluorescent derivatives extracted with chloroform and subsequently measured
at 600,580 and 580 nm after excitation at 520,455 and 490 nm for cefi, ceph and cefo respectively. The optimum experimental
conditions have been studied. Beer’s law is obeyed over the concentrations of 10–35 ng/mL, 10–60 ng/mL and 20–45 ng/mL for
cefi,ceph and cefo, respectively. The detection limits were 2.02 ng/mL, 2.09 ng/mL and 2.30 ng/mL for cefi, ceph and cefo,
respectively, with a linear regression correlation coefficient of 0.9987, 0.9995 and 0.9991 and recoveries in range from 98.5-107.04,
95.17-101.00 and 95.00-109.55% for cefi, ceph and cefo, respectively. This method is simple and can be applied for the determination
of cefi, ceph and cefo in pharmaceutical formulations in quality control laboratories. 相似文献
4.
Two simple, accurate and highly sensitive spectrofluorometric methods were developed for the determination of ethamsylate
(ETM). Method I is based on measuring the native fluorescence of ethamsylate in water at 354 nm after excitation at 302 nm.
The calibration plot was rectilinear over the range of 0.05–1 μg/mL for ETM with limits of detection and quantitation of 7.9
and 26 ng/mL, respectively. Method II involved synchronous and first derivative synchronous fluorometric methods for the simultaneous
determination of ethamsylate (ETM) and hydroquinone (HQ) which is considered as an impurity and/or acidic degradation product.
The synchronous fluorescence of both the drug and its impurity were measured in methanol at Δ λ of 40 nm. The peak amplitudes
(1D) were estimated at 293.85 or 334.17 nm for ETM and at 309.05 nm for HQ. Good linearity was obtained for ETM over the ranges
0.1–1.4 μg/mL and 0.1–1.0 μg/mL at 293.85 and 334.17 nm, respectively. For HQ, the calibration plot was rectilinear over the
range of 0.01–0.14 μg/mL at 309.05 nm. Limits of detection were 20, 2.01 ng/mL and limits of quantitation were 60, 6.7 ng/mL
for ETM and HQ by method II, respectively. Both methods were successfully applied to commercial ampoules and tablets. The
results were in good agreement with those obtained by the reference method. Method I was utilized to study the stability of
ETM and its degradation kinetics using peroxide. The apparent first-order rate constant, half-life times and activation energy
of the degradation process were calculated. Method I was further extended to the in-vitro and in-vivo determination of ETM
in spiked and real plasma samples. The mean% recoveries were 99.57 ± 3.85 and 89.39 ± 5.93 for spiked and real human plasma,
respectively. 相似文献
5.
A new spectrofluorimetric method has been developed and validated for the quantification of ceftriaxone in bulk powder, pharmaceutical
formulations and spiked human plasma. The developed method is reproducible, accurate, sensitive and cost effective. In this
method, ceftriaxone was converted into a fluorescent compound by reacting with 0.8 M ethyl acetoacetate and 25% formaldehyde
in a buffered medium (pH = 4.2) at 90 °C. The excitation and emission wavelengths of the fluorescent reaction product are
316 nm and 388 nm respectively. Optimization of the experimental conditions affecting the condensation reaction were carefully
carried out and the optimum experimental conditions were incorporated in the procedure. The developed method has a broad linear
range (0.2–20 μg mL−1) with a correlation coefficient of 0.9992. The limit of detection (LOD) and limit of quantification (LOQ) was found to be
1.94 × 10−2 μg mL−1 and 6.47 × 10−2 μg mL−1 respectively. The common excipients and co-administered drugs were investigated for their interferences effect in the assay.
The developed method was validated statistically through recovery studies and successfully applied to ceftriaxone determination
in bulk powder, pharmaceutical formulations and spiked human plasma samples. The percent recoveries were found to be in the
range of 99.04–100.26% for bulk powder, 98.88–99.92% for pharmaceutical formulations and 94.22–98.48% for spiked human plasma.
The results were verified by comparing with reference literature HPLC method and were found in good agreement. 相似文献
6.
A simple, economic, selective, and stability indicating spectrofluorimetric method was developed for the determination of
famotidine (FMT); is based on its reaction with 9, 10-phenanthraquinone in alkaline medium to give a highly fluorescent derivative
measured at 560 nm after excitation at 283 nm. The fluorescence intensity - concentration plot was rectilinear over the concentration
range of 50–600 ng/ml with minimum quantification limit (LOQ) of 13.0 ng/ml and minimum detection limit (LOD) of 4.3 ng/ml.
The factors affecting the development of the fluorescence intensity of the reaction product were carefully studied and optimized.
The method was applied for the determination of FMT in its dosage forms. The stability of the compound was studied, and the
proposed method was found to be stability indicating one. The results obtained were in good agreement with those obtained
by the official method. Furthermore, the method was applied for the determination of FMT in spiked and real human plasma.
The mean % recovery (n = 4) was found to be 99.94 ± 0.24, and 105.13 ± 0.64 for spiked and real human plasma, respectively. The composition of the
reaction product as well as its stability constant was also investigated. Moreover, the method was utilized to investigate
the kinetics of both alkaline and oxidative induced degradation of the drug. The apparent first order rate constant and half
life time of the degradation product was calculated. A proposal of the reaction pathway was postulated. 相似文献
7.
A simple, sensitive and rapid spectrofluorometric method for determination of methocarbamol in pharmaceutical formulations
and spiked human plasma has been developed. The proposed method is based on the measurement of the native fluorescence of
methocarbamol in methanol at 313 nm after excitation at 277 nm. The relative fluorescence intensity-concentration plot was
rectilinear over the range of 0.05–2.0 μg/mL, with good correlation (r = 0.9999), limit of detection of 0.007 μg/ mL and a lower limit of quantification of 0.022 μg/ mL. The described method was
successfully applied for the determination of methocarbamol in its tablets without interference from co-formulated drugs,
such as aspirin, diclofenac, paracetamol and ibuprofen, The results obtained were in good agreement with those obtained using
the official method (USP 30).The high sensitivity of the method allowed the determination of the studied drug in spiked human
plasma with average percentage recovery of 99.42 ± 3.84. 相似文献
8.
Adamou R Coly A Abdoulaye A Soumaila M Moussa I Ikhiri K Tine A 《Journal of fluorescence》2011,21(4):1409-1415
An analytical method based on the use of UV-irradiation to produce fluorescent derivatives from Etofenprox a non-fluorescent
pyrethroid insecticide is described. The impact of cetyltrimethylammonium chloride (CTAC) micellar medium on the Etofenprox
photochemically-induced fluorescence (PIF) is reported. Parameters influencing the sensitivity and repeatability of the PIF
method have been optimized. The alkaline medium (NaOH 6 × 10−2 M) + CTAC surfactant molecules (3.84 mg/ml) in acetonitrile is found to be very suitable for this pyrethroid insecticide
analysis in environment matrices. Linear dynamic range is established over more than two orders of magnitude. The limit of
detection is lower than 5 ng/ml. The method seems to be suitable for environmental matrices quality control. Application to
the analysis of spiked natural waters gave recoveries rate ranged from 94 to 104% and 107 to 115% respectively for river and
pound water. 相似文献
9.
A highly sensitive and simple spectrofluorimetric method has been developed and validated for the determination of the antidepressant
fluvoxamine (FXM) in its dosage forms and plasma. The method was based on nucleophilic substitution reaction of FXM with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole
in an alkaline medium (pH 8) to form a highly fluorescent derivative that was measured at 535 nm after excitation at 470 nm.
The factors affecting the reaction was carefully studied and optimized. The kinetics of the reaction was investigated, and
the reaction mechanism was presented. Under the optimized conditions, linear relationship with good correlation coefficient
(0.9995) was found between the fluorescence intensity and FXM concentration in the range of 65–800 ng ml−1. The limits of detection and quantitation for the method were 21 and 64 ng ml−1, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2.17%.
The proposed method was successfully applied to the determination of FXM in its pharmaceutical tablets with good accuracy;
the recovery values were 97.8–101.4 ± 1.08–2.75%. The results obtained by the proposed method were comparable with those obtained
by the official method. The high sensitivity of the method allowed its successful application to the analysis of FXM in spiked
human plasma. The proposed method is superior to the previously reported spectrofluorimetric method for determination of FXM
in terms of its simplicity. The proposed method is practical and valuable for its routine application in quality control and
clinical laboratories for analysis of FXM. 相似文献
10.
M. Walash M. Sharaf El-Din Nahed El-Enany M. Eid Sh. Shalan 《Journal of fluorescence》2010,20(6):1275-1285
A rapid, simple and highly sensitive first derivative synchronous fluorometric method has been developed for the simultaneous
analysis of binary mixture of sulpiride (SUL) and mebeverine hydrochloride (MEB). The method is based upon measurement of
the synchronous fluorescence intensity of these drugs at ∆λ = 100 nm in water. The different experimental parameters affecting
the fluorescence of the two drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear
over the range of 0.05–1 μg/mL and 0.2–3.2 μg/mL for SUL and MEB respectively with lower detection limits (LOD) of 0.006 and
0.01 μg/mL and quantification limits (LOQ) of 0.0.02 and 0.05 μg/mL for SUL and MEB, respectively. The proposed method was
successfully applied for the determination of the two compounds in synthetic mixtures and in commercial tablets. The high
sensitivity attained by the proposed method allowed the determination of both of SUL and MEB metabolite (veratic acid) in
real human plasma samples applying second derivative synchronous fluorometric technique. The mean% recoveries (n = 3) for both MEB metabolite (veratic acid) and SUL were 99.82 ± 2.53 and 98.84 ± 6.20 for spiked human plasma respectively,
while for real human plasma, the mean% recoveries (n = 3) were 91.49 ± 4.25 and 91.36 ± 8.46 respectively. 相似文献
11.
A simple, selective and sensitive luminescence method has been developed for the assay of etodolac (I), moxepril HCl (II)
and fexofenadine HCl (III) in bulk drug and pharmaceutical formulations. The method is based on the luminescence sensitization
of europium (Eu3+) by complexation with the studied drugs. The fluorescence intensities of the products were measured at 667 nm for (I) and
at 615 for (II) and (III) while exciting at 276 for all the studied drugs. The fluorescence intensity was directly proportional
to the concentration over the range (20–280), (40–240) and (30–80) ng/ml with limits of detection (LOD) = 0.93, 0.92 and 0.95 μg/ml
for drugs I, II and III respectively. Optimum conditions for the formation of the complex in methanol were carefully studied.
The proposed method was successfully applied for the assay of the studied drugs in pharmaceutical formulations with excellent
recovery. 相似文献
12.
Sevgi Tatar Ulu 《Optics and Spectroscopy》2011,110(4):508-512
Simple, rapid and highly sensitive spectrofluorimetric methods were developed for the determination of venlafaxine in pure
and pharmaceutical preparations. The proposed methods were based on the reaction of venlafaxine as n-electron donor with π-acceptors namely, p-bromanil and p-chloranil. The method for the determination of venlafaxine over a concentration range of 5–100 and 5–150 ng/mL, for p-bromanil and p-chloranil methods, respectively. The intra- and inter-day precisions were satisfactory, the relative standard deviations
did not exceed 1.69%. The proposed method was successfully applied to the determination of venlafaxine in its pharmaceutical
preparations with good accuracy; the mean recovery percentages were 99.80%. The results were compared favorably with those
of the reference method. 相似文献
13.
L Pei D Dai Y Bao F Chen J Zheng J Li S Liu X Chen 《Journal of mass spectrometry : JMS》2012,47(8):962-968
A sensitive rapid analytical method was established and validated to determine the bakkenolide A (BA) in rat plasma. This method was further applied to assess the pharmacokinetics of BA in rats receiving a single dose of BA. Liquid chromatography tandem mass spectrometry in multiple reaction monitoring mode was used in the method, and costundide was used as internal standard. A simple protein precipitation based on methanol was employed. The combination of a simple sample cleanup and short chromatographic running time (2.4?min) increased the throughput of the method substantially. The method was validated over the range of 1-1000?ng/mL with a correlation coefficient?>?0.99. The lower limit of quantification was 1?ng/mL for BA in plasma. Intra- and inter-day accuracies for BA were 93-112% and 103-104%, respectively, and the inter-day precision was less than 15%. After a single oral dose of 20?mg/kg of BA, the mean peak plasma concentration (C(max) ) of BA was 234.7?±?161?ng/mL at 0.25?h. The area under the plasma concentration-time curve (AUC(0-24 h) ) was 535.8?±?223.7?h·ng/mL, and the elimination half-life (T(1/2) ) was 5.0?±?0.36?h. In case of intravenous administration of BA at a dosage of 2?mg/kg, the area under the plasma concentration-time curve (AUC(0-24 h) ) was 342?±?98 h?ng/mL, and the elimination half-life (T(1/2) ) was 5.8?±?0.7?h. Based on the results, the oral bioavailability of BA in rats at 20?mg/kg is 15.7%. Copyright ? 2012 John Wiley & Sons, Ltd. 相似文献
14.
Nahed M. El-Enany Dina T. El-Sherbiny Amina A. Abdelal Fathalla F. Belal 《Journal of fluorescence》2010,20(2):463-472
A sensitive, simple and selective spectrofluorimetric method was developed for the determination of Lamotrigine (LMT) in pharmaceutical
formulations and biological fluids. The method is based on reaction of LMT with o-phthalaldehyde in presence of 2-mercaptoethanol in borate buffer of pH 9.8 to yield a highly fluorescent derivative that
is measured at 448 nm after excitation at 337 nm. The different experimental parameters affecting the development and stability
of the reaction product were carefully studied and optimized. The fluorescence-concentration plot was rectilinear over the
range of 0.1–1.0 μg ml−1 with lower limit of detection (LOD) 0.02 μg ml−1 and limit of quantification (LOQ) 0.06 μg ml−1 respectively. The proposed method was successfully applied to the the analysis of commercial tablets. Statistical comparison
of the results obtained by the proposed and reference method revealed no significant difference in the performance of the
two methods regarding the accuracy and precision respectively. The proposed method was further extended to the in-vitro and in-vivo determination of the drug in spiked and real human plasma. The mean percentage recoveries in spiked and real human plasma
(n = 3) were 95.78 ± 1.37 and 90.93 ± 2.34 respectively. Interference arising from co-administered drugs was also studied. A
proposal for the reaction pathway with o-phthalaldehyde was postulated. 相似文献
15.
M. S. Raghu K. Basavaiah P. J. Ramesh Sameer A. M. Abdulrahman K. B. Vinay 《Journal of Applied Spectroscopy》2012,79(1):131-138
A sensitive, precise, and cost-effective UV-spectrophotometric method is described for the determination of pheniramine maleate
(PAM) in bulk drug and tablets. The method is based on the measurement of absorbance of a PAM solution in 0.1 N HCl at 264 nm.
As per the International Conference on Harmonization (ICH) guidelines, the method was validated for linearity, accuracy, precision,
limits of detection (LOD) and quantification (LOQ), and robustness and ruggedness. A linear relationship between absorbance
and concentration of PAM in the range of 2–40 μg/ml with a correlation coefficient (r) of 0.9998 was obtained. The LOD and
LOQ values were found to be 0.18 and 0.39 μg/ml PAM, respectively. The precision of the method was satisfactory: the value
of relative standard deviation (RSD) did not exceed 3.47%. The proposed method was applied successfully to the determination
of PAM in tablets with good accuracy and precision. Percentages of the label claims ranged from 101.8 to 102.01% with the
standard deviation (SD) from 0.64 to 0.72%. The accuracy of the method was further ascertained by recovery studies via a standard
addition procedure. In addition, the forced degradation of PAM was conducted in accordance with the ICH guidelines. Acidic
and basic hydrolysis, thermal stress, peroxide, and photolytic degradation were used to assess the stability-indicating power
of the method. A substantial degradation was observed during oxidative and alkaline degradations. No degradation was observed
under other stress conditions. 相似文献
16.
A highly sensitive, simple and rapid spectrofluorimetric method was developed for the determination of Terbinafine HCl (TRH) and linezolid (LNZ) in their pharmaceutical formulations. The proposed method is based on measuring the native fluorescence of the studied drugs in water at 336 nm after excitation at 275 nm for TRH and 375 nm after excitation at 254 nm for LNZ. The fluorescence–concentration plots were rectilinear over the range of 0.02–0.15 μg/mL for TRH and 0.5–5.0 μg/mL for LNZ. With lower detection limits of 3.0 and 110.0 ng/mL and a lower quantification limit of 9.0 and 320.0 ng/mL for TRH and LNZ, respectively. The method was successfully applied to the analysis of TRH in its commercial tablets, cream, gel and spray formulations and the results were in good agreement with those obtained with the official method. In addition the method was also applied to the analysis of LNZ in its capsule and I.V solution and the results were in good agreement with those obtained with the comparison method. The effect of sensitizers was studied. The method was extended to the determination of the studied drugs in spiked human plasma and the results were satisfactory. 相似文献
17.
P. J. Ramesh K. Basavaiah N. Rajendraprasad O. Zenita Devi K. B. Vinay 《Journal of Applied Spectroscopy》2011,78(3):383-391
Two simple spectrophotometric methods have been developed to analyze ofloxacin (OFX) in pharmaceuticals. The methods are based
on the oxidation of OFX by a measured excess of cerium(IV) sulfate in H2SO4 medium. This was followed by the determination of the unreacted oxidant by reacting it with either p-toluidine (p-TD) and measuring the absorbance at 525 nm (method A) or o-dianisidine (o-DA) and measuring the absorbance at 470 nm (method B). In both methods, the amount of cerium(IV) sulfate reacted corresponds
to the amount of OFX. Calibration graphs were linear over the ranges of 0–120 and 0–4 g/ml OFX for methods A and B, respectively.
The calculated molar absorptivity (2.34⋅103 and 5.99⋅104), Sandell sensitivity, and limit of quantification for the methods are reported. The intra-day precision (%RSD) and accuracy
(%RE) were < 8.0 and ≤ 4.0%, respectively, and the inter-day RSD and RE values were within 5 and 4.0%, respectively. The applicability
of the methods was demonstrated by determining OFX in tablets with an accuracy (%RE) of < 3% and precision (%RSD) of ≤2.65%.
The accuracy of the methods was further ascertained by recovery experiments via a standard-addition procedure. 相似文献
18.
H. Y. Tsai C. Y. Chang Y. C. Li W. C. Chu K. Viswanathan C. Bor Fuh 《Journal of nanoparticle research》2011,13(6):2461-2467
We combined a sandwich immunoassay, anti-CEA/CEA/anti-CEA, with functional magnetic (~80 nm) and fluorescent (~180 nm) nanoparticles
in magnetic separators to demonstrate a detection method for carcinoembryonic antigen (CEA). Determination of CEA in serum
can be used in clinical diagnosis and monitoring of tumor-related diseases. The CEA concentrations in samples were deduced
and determined based on the reference plot using the measured fluorescent intensity of sandwich nanoparticles from the sample.
The linear range of CEA detection was from 18 ng/mL to 1.8 pg/mL. The detection limit of CEA was 1.8 pg/mL. In comparison
with most other detection methods, this method had advantages of lower detection limit and wider linear range. The recovery
was higher than 94%. The CEA concentrations of two serum samples were determined to be 9.0 and 55 ng/mL, which differed by
6.7% (9.6 ng/mL) and 9.1% (50 ng/mL) from the measurements of enzyme-linked immunosorbent assay (ELISA), respectively. The
analysis time can be reduced to one third of ELISA. This method has good potential for other biomarker detections and biochemical
applications. 相似文献
19.
20.
M. M. Seleim M. S. Abu-Bakr E. Y. Hashem A. M. El-Zohry 《Journal of Applied Spectroscopy》2009,76(4):554-563
A highly sensitive and selective first-derivative spectrophotometric method has been developed for the determination of aluminum
and iron in mixtures. The method is based on the formation of the binary complexes of aluminum and iron with Alizarin yellow
R (AYR) 5-[4-nitrophenylazo]salicylic acid at pH 2.0 with molar absorptivity of 1.1∙104 l⋅mol–1⋅cm–1. A zero-crossing technique is found suitable for the direct measurement of the first derivative value at the specified wavelength,
so aluminum and iron were thus determined in the ranges 1.3–5.4 μg/ml and 1.1–8.3 μg/ml, respectively, in the presence of
both components. The detection limits were found to be 1.4 ng/ml for aluminum and 2.8 ng/ml for iron. The relative standard
deviations were in all cases less than 1.5%. The proposed method was successfully applied for the simultaneous determination
of aluminum and iron in certified reference aluminum samples. 相似文献