scholarly journals Quantitative Analysis of Lorazepam in Pharmaceutical Formulation Through FTIR Spectroscopy

2012 ◽  
Vol 9 (4) ◽  
pp. 2232-2238 ◽  
Author(s):  
Elaheh Konoz ◽  
Amir Hossein Mohsen Sarrafi ◽  
Marjaneh Samadizadeh ◽  
Samaneh Boreiri
Keyword(s):  
Limit Of Detection ◽  
Direct Determination ◽  
Good Alternative ◽  
Peak Height ◽  
Pharmaceutical Products ◽  
Height Measurement ◽  
Line Extraction ◽  
Relative Standard ◽  
Standard Solution

A Fourier transform infrared (FTIR) spectrophotometric method was development for the rapid, direct measurement of lorazepam in different pharmaceutical products. The method involves the off-line extraction of lorazepam with sonication and direct determination in the extract through peak height measurement in the 1704 cm-1using a baseline correction between 1850 and 1550 cm-1. For standardization an external calibration line established from standard solutions of lorazepam in chloroform were used. The method provides a limit of detection of 0.0030 mg per tablet (n=5), a relative standard deviation (RSD) of 2.65% for 5 independent measurement of standard solution at a concentration level of 1 mgg-1. Result obtained by FTIR agrees with those obtained by a reference methodology based on ultraviolet spectrometry and thus the developed procedure offers a good alternative for the determination of lorazepam in commercial products.

scholarly journals Voltammetric Determination of Phenylalanine Using Chemically Modified Screen-Printed Based Sensors

Chemosensors ◽  
2020 ◽  
Vol 8 (4) ◽  
pp. 113
Author(s):  
Ancuta Dinu ◽  
Constantin Apetrei
Keyword(s):  
Prussian Blue ◽  
Direct Determination ◽  
Standard Addition ◽  
Pharmaceutical Products ◽  
Electrochemical Process ◽  
Pharmaceutical Samples ◽  
Analytical Recovery ◽  
Relative Standard ◽  
Screen Printed

This paper describes the sensitive properties of screen-printed carbon electrodes (SPCE) modified by using three different electroactive chemical compounds: Meldola’s Blue, Cobalt Phthalocyanine and Prussian Blue, respectively. It was demonstrated that the Prussian Blue (PB) modified SPCE presented electrochemical signals with the highest performances in terms of electrochemical process kinetics and sensitivity in all the solutions analyzed. PB-SPCE was demonstrated to detect Phe through the influence it exerts on the redox processes of PB. The PB-SPCE calibration have shown a linearity range of 0.33–14.5 µM, a detection limit (LOD) of 1.23 × 10−8 M and the standard deviation relative to 3%. The PB-SPCE sensor was used to determine Phe by means of calibration and standard addition techniques on pure samples, on simple pharmaceutical samples or on multicomponent pharmaceutical samples. Direct determination of the concentration of 4 × 10−6–5 × 10−5 M Phe in KCl solution showed that the analytical recovery falls in the range of 99.75–100.28%, and relative standard deviations in the range of 2.28–3.02%. The sensors were successfully applied to determine the Phe in pharmaceuticals. The validation of the method was performed by using the FTIR, and by comparing the results obtained by PB-SPCE in the analysis of three pharmaceutical products of different concentrations with those indicated by the producer.

Micellar-Enhanced Spectrofluorimetric Method for Quantification of Diclofenac Potassium in Pure Form, in Pharmaceutical Preparations and Human Plasma

2021 ◽  
Vol 58 (6) ◽  
pp. 427-434
Author(s):  
Muhammad Naeem Khan ◽  
Irum ◽  
Saba Gul ◽  
Muslima ◽  
Muhammad Mursaleen
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Pure Form ◽  
Fluorescence Signal ◽  
Spectrofluorimetric Method ◽  
Relative Standard

Abstract A rapid, simple and economical spectrofluorimetric method for the determination of diclofenac potassium in pure form, in pharmaceutical preparations and in human plasma has been developed. The method is based on the enhancement of the fluorescence signal of diclofenac potassium by the addition of sodium dodecyl sulphate in McIvaine buffer with a pH of 5. Different experimental conditions such as buffer type, pH, type and concentration of surfactants were investigated. The fluorescence intensity of the solution was recorded at 361 nm after excitation at 243 nm. The method shows linearity in the concentration range of 0.2 μg mL–1–10 μg mL–1 with a good correlation coefficient of 0.997. The relative standard deviation value was 3.62 (n = 7). The limit of detection and limit of quantification were calculated to be 2.84 × 10–3 μg mL–1 and 9.47 × 10–3 μg mL-1, respectively. The effect of excipients and co-administrated drugs was investigated and no interference was observed. The method was successfully applied for the determination of diclofenac potassium in pure form, in pharmaceutical products and in human plasma. The percentage recoveries obtained ranged from 100.25% to 102.16% for pure form and 97.50% to 102.00% for pharmaceutical products and from 98.50% to 101.67% for human plasma.

scholarly journals HPLC-DAD Determination of Iodide in Mineral Waters on Phosphatidylcholine Column

Molecules ◽  
2019 ◽  
Vol 24 (7) ◽  
pp. 1243 ◽  
Author(s):  
Małgorzata Tatarczak-Michalewska ◽  
Jolanta Flieger ◽  
Justyna Kawka ◽  
Wojciech Flieger ◽  
Eliza Blicharska
Keyword(s):  
Water Samples ◽  
Mineral Water ◽  
Limit Of Detection ◽  
Direct Determination ◽  
Sample Pretreatment ◽  
Calibration Graph ◽  
Mineral Waters ◽  
Independent Analysis ◽  
Relative Standard

Iodine is an essential nutrient necessary for the production of thyroid hormones. A valuable source of iodide, which is the bio-available iodine form could be mineral waters offered by different spas. In this work, the method capable of direct determination of iodide in mineral water samples based on IAM liquid chromatography on the phosphatidylcholine column (IAM.PC.DD2 Regis HPLC) with DAD detection without sample pretreatment or any pre-concentration steps is presented. The calibration graph for iodide was linear in the range of 0.5–10.0 mg L−1 with a correlation coefficient of 0.9996. The limit of detection was 22.84 ng mL−1. The relative recoveries were in the interval of 98.5–100.2% and the repeatability, expressed as a relative standard deviation (RSD) was less than 5%. The RSA (Response Surface Analysis) investigated the effect of the sample concentration and the injection volume. The iodide concentrations in the mineral water samples ranged from 0.58 to 2.88 mg L−1. The accuracy of the method was assessed through independent analysis by ICP-MS. Iodide levels measured by these two procedures did not significantly differ. The effects of interfering ions like HCO3−, Cl−, SO42−, F−, and Br− were also tested. The analysis has shown insignificant differences in the values of the iodide peak area and its height measured in multicomponent mixtures with an error smaller than 5%.

scholarly journals Spectrophotometric Indirect Determination of Captopril through Redox Reaction with n-bromosuccinimide and RB dye in Pharmaceutical Products

2020 ◽  
Vol 8 (2) ◽  
pp. 8-14
Author(s):  
Dashne M. Kokhasmail ◽  
Tara F. Tahir ◽  
Kurdistan F. Azeez
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Pharmaceutical Products ◽  
Indirect Determination ◽  
Relative Standard ◽  
Experimental Parameters ◽  
Replicated Measurements ◽  
Student’S T

A simple, accurate, and sensitive method for the spectrophotometric determination of captopril in bulk and dosage forms is reported. The method is based on the bromination of captopril with excess solution of n-bromosuccinimide (NBS) in HCl acid medium. The excess NBS is pursued by the assessment of the residual NBS based on its ability to bleach the rhodamine B dye and measuring the absorbance at 555 nm. The amount of NBS reacted coincides to the drug content. The different experimental parameters influencing the development and stability of the color are precisely studied and optimized. Beer’s law is valid within a concentration range of 0.3–1.0 μg/mL with a correlation coefficient R2 = 0.991. The limit of detection 0.169 μg/mL is attained and relative standard deviation values for five replicated measurements of 0.3, 0.7, and 1.0 μg/mL captopril were between 0.53% and 2.03%. No interference is detected from prevalent additives found in pharmaceutical preparations. The proposed method is profitably put on to the determination of captopril in the tablet formulations with mean recoveries 98.91–101.27% and the results were statistically confronted with those of a reference method by applying Student’s t-and F-test.

scholarly journals Photometric Determination of Iron in Pharmaceutical Formulations Using Double-Beam Direct Injection Flow Detector

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4498
Author(s):  
Stanislawa Koronkiewicz
Keyword(s):  
Flow System ◽  
Limit Of Detection ◽  
Direct Injection ◽  
Pharmaceutical Products ◽  
Complexing Agent ◽  
Photometric Detection ◽  
Relative Standard ◽  
Double Beam ◽  
Log Ratio

In this work, an innovative, flow-through, double-beam, photometric detector with direct injection of the reagents (double-DID) was used for the first time for the determination of iron in pharmaceuticals. For stable measurement of the absorbance, double paired emission-detection LED diodes and a log ratio precision amplifier have been applied. The detector was integrated with the system of solenoid micro-pumps. The micro-pumps helped to reduce the number of reagents used and are responsible for precise solution dispensing and propelling. The flow system is characterized by a high level of automation. The total iron was determined as a Fe(II) with photometric detection using 1,10-phenanthroline as a complexing agent. The optimum conditions of the propose analytical procedure were established and the method was validated. The calibration graph was linear in the range of 1 to 30 mg L−1. The limit of detection (LOD) was 0.5 mg L−1. The throughput of the method was 90 samples/hour. The repeatability of the method expressed as the relative standard deviation (R.S.D.) was 2% (n = 10). The method was characterized by very low consumption of reagents and samples (20 μL each) and a small amount of waste produced (about 540 µL per analysis). The proposed flow method was successfully applied for determination of iron in pharmaceutical products. The results were in good agreement with those obtained using the manual UV-Vis spectrophotometry and with values claimed by the manufacturers. The flow system worked very stably and was insensitive to bubbles appearing in the system.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

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.

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

scholarly journals Determination of cobalt in water samples by atomic absorption spectrometry after pre-concentration with a simple ionic liquid-based dispersive liquid-liquid micro-extraction methodology

2010 ◽  
Vol 8 (3) ◽  
pp. 617-625 ◽  
Author(s):  
Hossein Abdolmohammad-Zadeh ◽  
Elnaz Ebrahimzadeh
Keyword(s):  
Ionic Liquid ◽  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Water Samples ◽  
Limit Of Detection ◽  
Absorption Spectrometry ◽  
Experimental Conditions ◽  
Flame Atomic Absorption ◽  
Relative Standard

AbstractA rapid dispersive liquid-liquid micro-extraction (DLLME) methodology based on the application of 1-hexylpyridinium hexafluorophosphate [C6py][PF6] ionic liquid (IL) as an extractant solvent was applied for the pre-concentration of trace levels of cobalt prior to determination by flame atomic absorption spectrometry (FAAS). 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was employed as a chelator forming a Co-PMBP complex to extract cobalt ions from aqueous solution into the fine droplets of [C6py][PF6]. Some effective factors that influence the micro-extraction efficiency include the pH, the PMBP concentration, the amount of ionic liquid, the ionic strength, the temperature and the centrifugation time which were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enrichment factor were 0.70 µg L−1 and 60, respectively. The relative standard deviation (RSD) for six replicate determinations of 50 µg L−1 Co was 2.36%. The calibration graph using the pre-concentration system was linear at levels 2–166 µg L−1 with a correlation coefficient of 0.9982. The applicability of the proposed method was evaluated by the determination of trace amounts of cobalt in several water samples.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

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.

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