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 Azocasein Substrate for Determination of Proteolytic Activity: Reexamining a Traditional Method Using Bromelain Samples

2016 ◽  
Vol 2016 ◽  
pp. 1-6 ◽  
Author(s):  
Diego F. Coêlho ◽  
Thais Peron Saturnino ◽  
Fernanda Freitas Fernandes ◽  
Priscila Gava Mazzola ◽  
Edgar Silveira ◽  
...  
Keyword(s):  
Quality Control ◽  
Traditional Method ◽  
Reliable Method ◽  
Limit Of Detection ◽  
Standard Protocol ◽  
Mathematical Approach ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Selection Of

Given the importance of protease’s worldwide market, the determination of optimum conditions and the development of a standard protocol are critical during selection of a reliable method to determine its bioactivity. This paper uses quality control theory to validate a modified version of a method proposed by Charney and Tomarelli in 1947. The results obtained showed that using azocasein substrate bromelain had its optimum at 45°C and pH 9 (Glycine-NaOH 100 mM). We also quantified the limit of detection (LoD) and limit of quantification (LoQ) in the above-mentioned optimum (0.072 and 0.494 mg·mL−1of azocasein, resp.) and a calibration curve that correlates optical density with the amount of substrate digested. In all analysed samples, we observed a significant decrease in response after storage (around 17%), which suggests its use must be immediately after preparation. Thus, the protocol presented in this paper offers a significant improvement, given that subjective definitions are commonly used in the literature and this simple mathematical approach makes it clear and concise.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

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.

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.

Analysis of Synthetic Antioxidant in Food by Capillary Electrophoresis

2011 ◽  
Vol 361-363 ◽  
pp. 1855-1858 ◽  
Author(s):  
Qian Xiang ◽  
Ying Gao
Keyword(s):  
Capillary Electrophoresis ◽  
Amperometric Detection ◽  
Peak Height ◽  
Butylated Hydroxyanisole ◽  
Applied Potential ◽  
Synthetic Antioxidant ◽  
Separation Potential ◽  
Relative Standard ◽  
Capillary Electrophoretic

A capillary electrophoretic assay for determining synthetic antioxidant butylated hydroxyanisole in food has been developed. The extraction with 70% (v/v) methanol quantitatively extracted synthetic antioxidant. The separation was carried out by CZE using phosphate at a separation potential of 18 kV. Amperometric detection was achieved with an applied potential of 0.60 V. A linear relationship between the peak height and the concentration of the analyte was found in the range 1.8-180 µg/mL for BHA, with correlation coefficient of 0.994. The relative standard deviations of migration time and peak height were 0.19 and 5.3 %, respectively. The method developed was successfully applied for the determination of synthetic antioxidant butylated hydroxyanisole in food. Recovery of butylated hydroxyanisole was 93%.

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.

scholarly journals Determination of Sulpiride by Capillary Electrophoresis with End-Column Electrogenerated Chemiluminescence Detection

2002 ◽  
Vol 48 (7) ◽  
pp. 1049-1058 ◽  
Author(s):  
Jifeng Liu ◽  
Weidong Cao ◽  
Haibo Qiu ◽  
Xiuhua Sun ◽  
Xiurong Yang ◽  
...  
Keyword(s):  
Capillary Electrophoresis ◽  
Human Plasma ◽  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Fused Silica ◽  
Urine Samples ◽  
Electrogenerated Chemiluminescence ◽  
Driving Voltage

Abstract Background: Capillary electrophoresis (CE) with tris(2,2′-bipyridyl)ruthenium(II) [Ru(bpy)32+]-electrogenerated chemiluminescence (ECL) detection is a promising method for clinical analysis. In this study, a method combining CE with Ru(bpy)32+ ECL (CE-ECL) detection that can be applied to amine-containing clinical species was developed, and the performance of CE-ECL as a quantitative method for determination of sulpiride in human plasma or urine was evaluated. Methods: Sulpiride was separated by capillary zone electrophoresis in uncoated fused-silica capillaries [50 cm × 25 μm (i.d.)] filled with phosphate buffer (pH 8.0) and a driving voltage of +15 kV, with end-column Ru(bpy)32+ ECL detection. A platinum disc electrode was used as working electrode. Sulpiride in human plasma or urine samples (100 μL) was extracted by a double-step liquid-liquid extraction procedure, dried under nitrogen at 35 °C in a water bath, and reconstituted with 100 μL of filtered water. The extraction solvent was ethyl acetate–dichloromethane (5:1 by volume). Results: Under optimum conditions (pH 8.0 phosphate buffer, injection for 6 s at 10 kV, and +1.2 V as detection potential), separation of sulpiride was accomplished within 4 min. The calibration curve was linear over a concentration range of 0.05–25.0 μmol/L, and the limit of detection was 2.9 × 10−8 mol/L for sulpiride. Intra- and interday CVs for ECL intensities were <6%. Extraction recoveries of sulpiride were 95.6–101% with CVs of 2.9–6.0%. The method was clinically validated for patient plasma and urine samples. Conclusions: CE combined with Ru(bpy)32+ ECL is reproducible, precise, selective, and enables the analysis of sulpiride in human plasma and urine. It thus is of value for rapid and efficient analysis of amine-containing analytes of clinical interest.

scholarly journals New Poly(Ionic Liquid) Based Fiber for Determination of Oxytetracycline in Milk Samples by Application of SPME-CE Technique

Molecules ◽  
2019 ◽  
Vol 24 (3) ◽  
pp. 430 ◽  
Author(s):  
T. Alexandra Ferreira ◽  
J. Francisco Flores-Aguilar ◽  
Eva M. Santos ◽  
Jose A. Rodriguez ◽  
Israel S. Ibarra
Keyword(s):  
Capillary Electrophoresis ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Ionic Exchange ◽  
Imidazolium Chloride ◽  
Milk Samples ◽  
Multi Stage ◽  
Pre Treatment ◽  
Poly Ionic Liquid

In this work, a procedure using solid phase microextraction in combination with capillary electrophoresis was developed for the determination of oxytetracycline in milk samples. The method involves the synthesis of poly(1-allyl-3-methyl imidazolium) chloride film on a stainless-steel bar via electropolymerization and its use as an adsorbent for oxytetracycline (OT) by an ionic exchange mechanism. The coated fiber is then immersed in milk samples for retention of oxytetracycline residues, followed by elution, drying, and reconstitution before analysis with capillary electrophoresis. The proposed method achieves a limit of detection of 70 µg L–1 with adequate precision and uncertainty, making this methodology appropriate for the determination of OT in milk samples. The method was applied to the pre-concentration and quantification of oxytetracycline in ten commercial milk samples. Two tested samples were positive for the presence of oxytetracycline but the concentration was below the maximum residue limit according to the international normative standard. The proposed methodology was evaluated according to the Eco-Scale approach, and the total score of 51 indicated that the methodology proposed is both green and acceptable despite the multi-stage character. SPME-CE methodology allows us to perform the sample pre-treatment and determination of OT in an effective and greener way, decreasing the number of steps during the analysis and the generation of waste.

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.

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