scholarly journals Development of CE-C4D Method for Determination Tropane Alkaloids

Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5749
Author(s):  
Małgorzata Gołąb ◽  
Martyna Przybyłowska ◽  
Petr Kubáň ◽  
Petra Itterheimová ◽  
Michał Woźniakiewicz
Keyword(s):  
Acetic Acid ◽  
Plant Extracts ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Tropane Alkaloids ◽  
Fast Method ◽  
Capacitively Coupled ◽  
Solanaceae Family ◽  
Detection And Quantification

A fast method for the determination of tropane alkaloids, using a portable CE instrument with a capacitively coupled contactless conductivity detector (CE-C4D) was developed and validated for determination of atropine and scopolamine in seeds from Solanaceae family plants. Separation was obtained within 5 min, using an optimized background electrolyte consisting of 0.5 M acetic acid with 0.25% (w/v) β-CD. The limit of detection and quantification was 0.5 µg/mL and 1.5 µg/mL, respectively, for both atropine and scopolamine. The developed method was validated with the following parameters—precision (CV): 1.07–2.08%, accuracy of the assay (recovery, RE): 101.0–102.7% and matrix effect (ME): 92.99–94.23%. Moreover, the optimized CE-C4D method was applied to the analysis of plant extracts and pharmaceuticals, proving its applicability and accuracy.

Fast Method for the Determination of Residual Solvents in Radiopharmaceutical Products

2017 ◽  
Vol 68 (4) ◽  
pp. 666-670 ◽  
Author(s):  
Mirela Mihon ◽  
Catalin Stelian Tuta ◽  
Alina Catrinel Ion ◽  
Dana Niculae ◽  
Vasile Lavric
Keyword(s):  
Gas Chromatography ◽  
Control Method ◽  
Limit Of Detection ◽  
The Body ◽  
Biologically Active ◽  
Injection Technique ◽  
Fast Method ◽  
Residual Solvent ◽  
Residual Solvents

The aim of this work was the development and validation of a fast analytical method to determine the residual solvents content in radiopharmaceuticals such as: 18F-Fluorodeoxyglucose (18F-FDG), 18F-Fluoroestradiol (18F-FES), 18F-Fluorothymidine (18F-FLT),18F-Fluoromisonidazole (18F-FMISO). Radiopharmaceuticals are radioactive preparations for medical purposes used in nuclear medicine as tracers in diagnostic imaging and treatment of certain diseases. Positron Emission Tomography (PET) is a medical imaging technique that consists in introducing into the body of a small amount of a biologically active chemical compound labelled with a short lived positron-emitting radioisotope (18F, 11C, 68Ga). Residual solvents are critical impurities in radiopharmaceuticals that can affect labelling, stability and physicochemical properties of drugs. Therefore, the determination of these solvents is essential for quality control of radiopharmaceuticals. Validation of the control method for residual solvents by gas chromatography is referred by the European Pharmacopoeia using a special injection technique (head space). The parameters of the method, which comply with International Conference on Harmonization guidelines, are: accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The proposed method (direct gas chromatography injection) proved to be linear, precise, accurate and robust. Good linearity was achieved for all the solvents and correlation coefficients (R2) for each residual solvent were found more than 0.99.

Reliable Method for the Determination of Food Additive by Capillary Electrophoresis Using a Microvolume of Foodstuffs

2011 ◽  
Vol 361-363 ◽  
pp. 1486-1489
Author(s):  
Qian Xiang ◽  
Ying Gao
Keyword(s):  
Capillary Electrophoresis ◽  
Reliable Method ◽  
Lower Cost ◽  
Limit Of Detection ◽  
Food Additive ◽  
Fast Method ◽  
Optimum Conditions ◽  
Applied Potential ◽  
Minimal Sample

A fast method for the separation and determination of the food additive propyl gallate has been established by using capillary electrophoresis. The effects of several factors such as the applied potential and detection running buffer were investigated in order to obtain the optimum conditions, and the assay results were satisfactory. The limit of detection for the analyte was 10-6 mol/L. This approach has remarkable advantages with respect to other methodologies involving separations and electrochemical detection including minimal sample consumption, higher analysis speed and lower cost. In order to demonstrate the capabilitiy of the method, the determination of additive in a commercial food sample is also presented.

scholarly journals Analysis of Seven Biogenic Amines and Two Amino Acids in Wines Using Micellar Electrokinetic Chromatography

2019 ◽  
Vol 9 (6) ◽  
pp. 1193 ◽  
Author(s):  
Chih-Ying Huang ◽  
Yu-Xian Wang ◽  
Xin-Zhi Wang ◽  
Cho-Chun Hu ◽  
Tai-Chia Chiu
Keyword(s):  
Amino Acids ◽  
Biogenic Amines ◽  
Micellar Electrokinetic Chromatography ◽  
Low Cost ◽  
Background Electrolyte ◽  
Sodium Dodecyl ◽  
Fast Method ◽  
Electrokinetic Chromatography ◽  
Optimal Separation

A low-cost, simple, and fast method utilizing micellar electrokinetic chromatography for the simultaneous determination of seven biogenic amines and two amino acids was developed. A background electrolyte containing 5 mM phosphate buffer (pH 3.7) and 20 mM sodium dodecyl sulfate was used. The optimal separation of nine investigated analytes was achieved in 11 min, with limits of detection (S/N = 3) ranging from 0.11 to 0.61 µM. The linear ranges for all analytes were observed between 0.55 and 10.0 μM (R2 > 0.990). The developed approach was extended to the analysis of analytes in commercial wine and beer samples. The recoveries of the proposed method ranged from 98.8% to 115.6%.

Thin Layer Chromatographic Determination of Citrinin

1979 ◽  
Vol 62 (1) ◽  
pp. 201-202 ◽  
Author(s):  
Robert D Stubblefield
Keyword(s):  
Acetic Acid ◽  
Thin Layer ◽  
Linear Relationship ◽  
Silica Gel ◽  
Coefficient Of Variation ◽  
Ethylenediaminetetraacetic Acid ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Tlc Plates

Abstract Clearly defined zones of citrinin can be obtained on thin layer chromatographic (TLC) plates and measured by fluorodensitometry. Silica gel plates were prepared as a slurry with aqueous 0.05M Na2EDTA (ethylenediaminetetraacetic acid), spread at 0.5 mm wet thickness, and activated at 105°C for 1 hr. Plates were developed in acetic acid-benzene (5+95). The limit of detection was 10 ng citrinin/zone. Densitometric analysis (365 nm excitation, 505 nm emission) revealed that a linear relationship exists for levels of 10 ng to at least 100 ng/zone wtih a coefficient of variation of ±5%.

scholarly journals Sensitive Spectrophotometric Determinations of Paracetamol and Protriptyline HCl Using 3-Chloro-7-hydroxy-4-methyl-2H-chromen-2-one

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Kumble Divya ◽  
Badiadka Narayana ◽  
Majal Sapnakumari
Keyword(s):  
Charge Transfer ◽  
Spectrophotometric Method ◽  
Charge Transfer Complex ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Pharmaceutical Samples ◽  
Chromogenic Reagent ◽  
Detection And Quantification

A new spectrophotometric method is developed for the determination of Paracetamol (PCT) and protriptyline HCl (PTP) in pure forms and in pharmaceutical formulations. The experiment involves the use of 3-chloro-7-hydroxy-4-methyl-2H-chromen-2-one as a novel chromogenic reagent for the determination of PCT and PTP. The method is based on the formation of charge transfer complex between the drugs and chromogenic reagent. Beer's law is obeyed in the concentration ranges 10.00–60.00 µg mL−1 for PCT at 545 nm and 40.00–160.00 µg mL−1 for PTP at 468 nm. The molar absorptivity, Sandell, sensitivity, and limit of detection and quantification are also calculated. The method has been successfully applied for the determination of both PCT and PTP in pharmaceutical samples with acceptable results.

scholarly journals ANALYTICAL METHOD VALIDATION OF ICP-AES FOR ANALYSIS OF CADMIUM, CHROMIUM, CUPRUM, MANGAN AND NICKEL IN MILK

2019 ◽  
pp. 341-344
Author(s):  
DAVID ALEXANDER ◽  
Abdul Rohman
Keyword(s):  
Heavy Metals ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Official Method ◽  
Fast Method ◽  
Limit Of Quantification ◽  
Milk Products ◽  
Relative Standard ◽  
Validation Parameters

Objective: The aim of this research was to validate inductively coupled plasma-atomic emission spectroscopy (ICP-AES) for quantitative analysis of cadmium (Cd), chromium (Cr), cuprum (Cu), mangan (Mn) and nickel (Ni) in milk products. Methods: The heavy metals in milk were determined using ICP-AES at optimized wavelength. The method was validated by assessing several validation parameters which included linearity and range, accuracy, precision and sensitivity expressed by the limit of detection and limit of quantification. The validated method was then used for the analysis of milks commercially available. Results: ICP-AES for determination of Cd, Cr, Cu, Mn, and Ni was linear over a certain concentration range with a coefficient correlation value of>0.997. The limit of quantification values of Cd, Cr, Cu, Mn, and Ni were 0.0047; 0.0050; 0.0066; 0.0061; and 0.0169 µg/ml, respectively. The precision of analytical method exhibited relative standard deviation (RSD) values of 3.18%; 4.17%; 3.05%; 2.93%; and 4.47% during repeatability test and 5.28%; 5.06%; 3.67%; 3.67%; and 11.17% during intermediate precision of Cd, Cr, Cu, Mn, and Ni respectively. The recoveries of these metals assessed using standard addition method were 92.25; 90.88; 102.87; 94.50; and 86.85%, respectively. Conclusion: ICP-AES offered a reliable and fast method for the determination of heavy metals in milk products. The developed method could be proposed as an official method for determination of heavy metals in milk products.

Simple and Fast Determination of Terbinafine in Human Urine by Dilute and Shoot HPLC-DAD Using a Core-Shell Column

2020 ◽  
Vol 23 ◽  
Author(s):  
Sercan Yıldırım ◽  
Gökhan Demirdaş ◽  
Mert Fidan ◽  
Ahmet Yaşar
Keyword(s):  
Flow Rate ◽  
Human Urine ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Therapeutic Drug ◽  
Core Shell ◽  
Pharmacokinetic Studies ◽  
Fast Method ◽  
Fast Determination

Background: Terbinafine is an allylamine antifungal which is effective against many fungi, dermatophytes and moulds. Analytical methods are required for the determination of terbinafine in biological fluids to perform therapeutic drug monitoring and pharmacokinetic studies. Objective: The aim of this study was to develop and validate a novel and fast method combining dilute and shoot approach and high-performance liquid chromatography coupled with photodiode array detection for the determination of terbinafine in human urine. Methods: Chromatographic parameters including mobile phase composition, pH, flow rate and injection volume was assessed and optimized. The separation of terbinafine and naproxen (internal standard) was achieved within 3 min using a C18 core-shell column (Raptor ARC-18, 100 x 4.6 mm, 2.7 µm) under isocratic conditions. Samples were eluted from the column at the flow rate of 1.4 mL/min using a mobile phase containing 0.2% triethylamine in water (pH 3.4 with formic acid): acetonitrile (45:55, v/v). Results: Presented technique was linear in the range of 25-2000 ng/mL. Intra- and inter-day reproducibility at four quality control levels (25, 200, 750 and 1500 ng/mL) was less than 7%, with relative errors ranging from -5.40% to 5.91%. Limit of detection was 12.60 ng/mL. Developed method has three main advantages compared to existing methods: simplicity and greenness of sample preparation, use of core-shell column and short analysis time. Conclusion: The results of this study indicate that the combination of dilute and shoot approach and core-shell column can be regarded as an advantageous application for the fast determination of terbinafine in urine.

Determination of Phenicols Using a Fast and Reliable HPLC Method Developed on Hypercarb Stationary Phase

2017 ◽  
Vol 68 (3) ◽  
pp. 545-548
Author(s):  
Georgeta Simona Stan ◽  
Florentina Moldovanu ◽  
Irinel Adriana Badea
Keyword(s):  
Stationary Phase ◽  
Mobile Phase ◽  
Reliable Method ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Detection Capability ◽  
Milk Samples ◽  
Precision And Accuracy ◽  
Detection And Quantification

Hypercarb porous graphitic stationary phase was used to develop a fast and reliable method for simultaneous determination of chloramphenicol, thiamphenicol and florfenicol. The separation was achieved in 7 min elution being made isocratic using water modified with acetonitrile as mobile phase. The method was fully validated and showed good linearity, precision and accuracy. Limit of detection and quantification together with decision limit and detection capability were established. This method was applied for analysis of milk samples.

scholarly journals A simple method for determination of deoxynivalenol in cereals and flours

2011 ◽  
Vol 20 (No. 2) ◽  
pp. 63-68 ◽  
Author(s):  
F. Kotal ◽  
Z. Radová
Keyword(s):  
Regression Analysis ◽  
Standard Deviation ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Fast Method ◽  
Immunoaffinity Column ◽  
Simple Method ◽  
Relative Standard ◽  
Certified Value

An effective and fast method for determination of deoxynivalenol (DON) in cereals and flours has been developed. The immunoaffinity column was used for the isolation of DON from wheat, corn, rice and flour extract. The determination was carried out by using the HPLC/UV method. The limit of detection was 0.02 mg/kg. The recoveries for the assay range 0.1 to 2 mg/kg were generally higher than 80%, ranging from 83 to 96% with an average relative standard deviation of 3.8%. The trueness of the method using the DON test – HPLC column was established by use of certified reference material CRM 379. The certified value was 0.67 mg/kg. The result obtained from three replicates was 0.68 ± 0.05 mg/kg. The corresponding confidence interval at 95% probability ranged from 0.63 to 0.73 mg/kg. A comparative study of the DON testTM – HPLC/UV and the Mycosep 225 – GC/ECD methods was carried out. Six naturally contaminated wheat samples were analysed by both methods. Linear regression analysis demonstrates that DON testTM – HPLC is a statistically significant predictor of the GC/ECD method using the Romer Mycosep 225 column.  

Determination of Intact Heparin by Capillary Electrophoresis with Contactless Conductivity Detection in Background Electrolytes Containing Hydrophilic Polymers

2008 ◽  
Vol 73 (2) ◽  
pp. 187-200 ◽  
Author(s):  
Petr Tůma ◽  
Eva Samcová ◽  
František Opekar ◽  
Karel Štulík
Keyword(s):  
Capillary Electrophoresis ◽  
Blood Plasma ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Inorganic Ions ◽  
Hydroxyethyl Cellulose ◽  
Conductivity Detection ◽  
Contactless Conductivity Detection ◽  
In Blood Plasma

Intact heparin was characterized and determined in model samples, in infusion solutions and in blood plasma by capillary electrophoresis (CE) with contactless conductivity detection. The CE separation of polydisperse heparin took place in open silica capillaries, in electrolytes containing a polymer (hydroxyethyl)cellulose, poly(ethylene glycol) or dextran. The best separation of heparin from excess inorganic ions present in real samples was attained in a background electrolyte consisting of 0.8 M acetic acid and 1% (w/v) dextran (100 kDa). The limit of detection (LOD) was 1.3 μmol l-1. This electrolyte was used in determination of heparin in blood plasma and in infusion solutions.

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