scholarly journals Determination of Calibration Characteristics of X-Ray Fluorescent Analysis of Rhenium

2010 ◽  
Vol 13 (3-4) ◽  
pp. 247
Author(s):  
Anna V. Troeglazova ◽  
Elena V. Zlobina ◽  
Alexander Yu. Sokolov ◽  
Anargul K. Zhangalieva

Extraction concentration of rhenium by a melt of tetraoctylammonium bromide in paraffin was used with the aim of preparation of calibration samples for roentgen fluorescent analysis. The calibration characteristics of the roentgen fluorescent analysis of rhenium is established, its linearity is evaluated, a limit of detection and a limit of quantification (determination) of rhenium are calculated. The maximal<br />value of the relative total standard uncertainty of the calibration characteristic does not exceed 1.45 %.

Nanomaterials ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 1650
Author(s):  
Gustavo Richter Vaz ◽  
Adryana Clementino ◽  
Juliana Bidone ◽  
Marcos Antonio Villetti ◽  
Mariana Falkembach ◽  
...  

Biphasic oil/water nanoemulsions have been proposed as delivery systems for the intranasal administration of curcumin (CUR) and quercetin (QU), due to their high drug entrapment efficiency, the possibility of simultaneous drug administration and protection of the encapsulated compounds from degradation. To better understand the physicochemical and biological performance of the selected formulation simultaneously co-encapsulating CUR and QU, a stability test of the compound mixture was firstly carried out using X-ray powder diffraction and thermal analyses, such as differential scanning calorimetry (DSC) and thermogravimetric analyses (TGA). The determination and quantification of the encapsulated active compounds were then carried out being an essential parameter for the development of innovative nanomedicines. Thus, a new HPLC–UV/Vis method for the simultaneous determination of CUR and QU in the nanoemulsions was developed and validated. The X-ray diffraction analyses demonstrated that no interaction between the mixture of active ingredients, if any, is strong enough to take place in the solid state. Moreover, the thermal analysis demonstrated that the CUR and QU are stable in the nanoemulsion production temperature range. The proposed analytical method for the simultaneous quantification of the two actives was selective and linear for both compounds in the range of 0.5–12.5 µg/mL (R2 > 0.9997), precise (RSD below 3%), robust and accurate (recovery 100 ± 5 %). The method was validated in accordance with ICH Q2 R1 “Validation of Analytical Procedures” and CDER-FDA “Validation of chromatographic methods” guideline. Furthermore, the low limit of detection (LOD 0.005 µg/mL for CUR and 0.14 µg/mL for QU) and the low limit of quantification (LOQ 0.017 µg/mL for CUR and 0.48 µg/mL for QU) of the method were suitable for the application to drug release and permeation studies planned for the development of the nanoemulsions. The method was then applied for the determination of nanoemulsions CUR and QU encapsulation efficiencies (> 99%), as well as for the stability studies of the two compounds in simulated biological fluids over time. The proposed method represents, to our knowledge, the only method for the simultaneous quantification of CUR and QU in nanoemulsions.


Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.


Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>


1974 ◽  
Vol 23 (4) ◽  
pp. 333-339
Author(s):  
Hideki TANAKA ◽  
Tomio OZAKI ◽  
Yuzo MORIGUCHI ◽  
Hiroyuki KITAMURA ◽  
Genzo HASHIZUMF
Keyword(s):  
X Ray ◽  

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.


2012 ◽  
Vol 2012 ◽  
pp. 1-6
Author(s):  
S. N. Prashanth ◽  
Shankara S. Kalanur ◽  
Nagappa L. Teradal ◽  
J. Seetharamappa

The electrochemical behavior of isothipendyl hydrochloride (IPH) was investigated at bare and multiwalled-carbon-nanotube modified glassy carbon electrode (MWCNT-GCE). IPH (55 μM) showed two oxidation peaks in Britton-Robinson (BR) buffer of pH 7.0. The oxidation process of IPH was observed to be irreversible over the pH range of 2.5–9.0. The influence of pH, scan rate, and concentration of the drug on anodic peak was studied. A differential pulse voltammetric method with good precision and accuracy was developed for the determination of IPH in pure and biological fluids. The peak current was found to be linearly dependent on the concentration of IPH in the range of 1.25–55 μM. The values of limit of detection and limit of quantification were noticed to be 0.284 and 0.949 μM, respectively.


Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (06) ◽  
pp. 60-63
Author(s):  
Sadhana Rajput ◽  
◽  
Samir Patel ◽  

A new, specific, selective, simple, rapid and inexpensive spectrofluorophotometric method has been developed for the determination of tadalafil in spiked human plasma. The fluorescence spectrum of tadalafil in 0.1M methanolic sulphuric acid showed excitation wavelength at 315 nm and emission wave-length at 332 nm. The method for tadalafil was found to be linear over the concentration range of 10-50 ng/mL with a correlation coefficient of 0.9991. Limit of detection and limit of quantification were found to be 0.235 ng/mL and 0.701 ng/mL, respectively. The method was validated and found to be suitable for the estimation of tadalafil from human plasma. Satisfactory recovery of tadalafil from the human plasma suggests no interference of any debris present into human plasma. This method can be used to deter-mine plasma tadalafil concentration in drug monitoring or pharmacokinetic investigation.


2019 ◽  
Vol 31 (1) ◽  
pp. 1-9
Author(s):  
Deepak Kumar Sahu ◽  
Joyce Rai ◽  
Chhaya Bhatt ◽  
Manish K. Rai ◽  
Jyoti Goswami ◽  
...  

In modern age pesticide is used widely in agriculture. Lambda-cyhalothrin (LCT) is one of the most used pesticides which are used as a insecticide to kill pest, tricks, flies etc in agricultural field and it is also used for crop production. We have developed new method to detect LCT insecticide in agriculture field and reduce its uses. In this method we found the maximum absorbance at 460 nm for yellow colour dye. We also calculated limit of detection and limit of quantification 0.001 mg kg-1 and 0.056 mg kg-1 respectively. Molar absorptivity and Sandell’s sensitivity was also calculated and obtained 1.782 ×107 mol-1 cm-1 and 9.996 ×10-6 µg cm-2 respectively. The obtained yellow colour dye obeyed Beer’s law limit range of 0.5 µg ml -1 to 16 µg ml-1 in 25 ml. This method is less time consuming, selective, simple, sensitive and low cost. Present method is successfully applied in various soil, water and vegetable samples.


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