scholarly journals HPLC separation and determination of dicoumarol and other simple coumarins in sweet clover

2018 ◽  
Vol 17 (1) ◽  
pp. 95-102 ◽  
Author(s):  
Katarína Hroboňová ◽  
Jana Sádecká ◽  
Jozef Čižmárik
Keyword(s):  
Fluorescence Spectra ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Excitation Wavelength ◽  
Sweet Clover ◽  
System Suitability ◽  
Synchronous Fluorescence Spectra ◽  
Peak Areas ◽  
Microbial Action

AbstractDicoumarol is a mycotoxin, that acts as a blood anticoagulant, is formed during the microbial action of molds and fungi in spoiled hay or silage containing high-coumarin plant. A HPLC-DAD method for determination of coumarins, including dicoumarol, coumarin, and 4-hydroxycoumarin was developed. Methanol and acetic acid were used as mobile phase with gradient elution. The simultaneous separation was performed using C18 type of stationary phase. The recoveries were 88.6 – 92.6 %, 91.8 – 95.0 %, and 89.7 – 94.1 % (evaluated for three concentration levels) for dicoumarol, coumarin, and 4-hydroxycoumarin respectively. The parameters of system suitability (repeatability of retention times and peak areas) were determined for evaluation of the method. The method showed a good linearity in the concentration range 0.7 – 100 μg.mL−1for dicoumarol, 0.05 – 100 μg.mL−1for coumarin and 4-hydroxycoumarin with correlation coefficients higher than 0.9885. Extracts of sweet clover herb, hay, and spoiled hay were subjected to HPLC-DAD analysis. The most abundant compound in sweet clover herb and hay extracts was coumarin. In spoiled sweet clover hay extract the 4-hydroxycoumarin was detected in addition. The formation of 4-hydroxycoumarin was also observed in the synchronous fluorescence spectra recorded at the wavelength difference of 90 nm (difference between emission and excitation wavelength).

scholarly journals Determination of adulterants in adulterant-fruit spirit blends using excitation-emission matrix fluorescence spectroscopy

2015 ◽  
Vol 8 (1) ◽  
pp. 52-58 ◽  
Author(s):  
Michaela Jakubíková ◽  
Jana Sádecká ◽  
Pavel Májek
Keyword(s):  
Wavelength Range ◽  
Fluorescence Spectra ◽  
Reliable Method ◽  
Excitation Wavelength ◽  
Mean Square ◽  
Excitation Emission Matrix ◽  
Ethanol Level ◽  
Parallel Factor ◽  
Eem Fluorescence

Abstract This study introduces a reliable method to detect adulteration of spirit drinks. Excitation-emission matrix (EEM) fluorescence in combination with parallel factor analysis (PARAFAC) and partial least squares (PLS) regression was used to determine the content of water and ethanol in adulterated fruit spirit samples. EEM fluorescence spectra recorded in the emission wavelength range of 315–450 nm and in the excitation wavelength range of 240–305 nm were used for PARAFAC. The model created using PARAFAC-PLS was able to predict the water and ethanol level in adulterated apple spirit with the root mean square error of prediction (RMSEP) values of 1.9 % and 1.8 %, respectively. Regarding adulterated plum spirit, the RMSEP values of 0.7 % and 3.5 % were obtained for water and ethanol, respectively. The aim of this work was to determine whether EEM-PARAFAC can be used to distinguish between plum and apple spirit. Better results were obtained for apple spirit and the method is useful also for water-apple spirit blends.

scholarly journals A reliable HPLC-DAD method for simultaneous determination of related substances in TBI-166 active pharmaceutical ingredient

2020 ◽  
Vol 32 (2) ◽  
pp. 80-85
Author(s):  
Tingting Zhang ◽  
Wanting Yin ◽  
Bo Jin ◽  
Tong Li ◽  
Chen Ma
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Active Pharmaceutical Ingredient ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Phase System ◽  
Related Substances ◽  
Ich Guidelines ◽  
Bulk Drug

A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

Determination of Gentamicin Residual in Duck Meat Using Fluorescence Analysis Method

2014 ◽  
Vol 1033-1034 ◽  
pp. 638-642
Author(s):  
Xiao Wang ◽  
Jiang Xu ◽  
Mu Hua Liu ◽  
Jin Hui Zhao ◽  
Qian Hong
Keyword(s):  
Correlation Coefficient ◽  
Fluorescence Spectra ◽  
Limit Of Detection ◽  
Fluorescence Analysis ◽  
Excitation Wavelength ◽  
Analysis Method ◽  
Standard Samples ◽  
Meat Extract ◽  
Coefficient Of Regression

Gentamicin is a kind of aminoglycoside antibiotics and widely used in the prevention and treatment of the duck diseases. A prediction model was established for the rapid detection of Gentamicin residue in duck meat using fluorescence analysis method according to the strong fluorescent characteristic of the generated derivative for Gentamicin and o-phthaldialdehyde (OPA) in the presence of emulsifier OP-10 and mercaptoethanol.The fluorescence spectra of the duck meat containing Gentamicin were analyzed, the optimum excitation wavelength of the material was 340 nm and the optimum emission wavelength was 442 nm. Fluorescence intensity and the concentration of the standard samples presented the good linear relationship, the linear correlation coefficient was 0.9963 and the limit of detection was 0.47 μg/mL in the dynamic rang of 0.5 ~6.5μg/mL. The correlation coefficient of regression equation was 0.9968 for the samples of duck meat extract. The experimental results showed that the fluorescence analysis method had a good performance and accuracy in detecting the Gentamicin residue in duck meat.

scholarly journals A Validated UPLC-PDA Method for Simultaneous Determination of 3 Biologically Active Isoflavans in Trigonella stellata Extract

2020 ◽  
Vol 15 (7) ◽  
pp. 1934578X2094011
Author(s):  
Safa M. Shams Eldin ◽  
Mohamed M. Radwan ◽  
Amira S. Wanas ◽  
Abdel-Azim M. Habib ◽  
Fahima F. Kassem ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Biologically Active ◽  
External Standard Method ◽  
Acid Aqueous Solution ◽  
Acquity Uplc

In this study, an ultra-performance liquid chromatography (UPLC)/photodiode array method was developed for the simultaneous determination of trigonellan glucoside (1), isotrigonellan (2), and methoxy-isotrigonellan (3) in Trigonella stellata extract using an external standard method. The extract was prepared using a standardized method by maceration of the dried plant material in ethanol. The 3 isoflavans (1-3) were separated on an Acquity UPLC C18 column using gradient elution with a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and 0.1% (v/v) formic acid in acetonitrile, and ultraviolet detection. The method provides a linear correlation for all analytes over the investigated ranges with all correlation coefficients greater than 0.998. The validated lower limits of quantitation were 53, 127, and 5 μg/mL for isoflavans 1, 2, and 3, respectively. Intraday and interday precisions (percent relative SD [RSD%]) were less than 8.3% and accuracy (RE%) ranged from 90% to 100%. The method’s capability to remain unaffected by small, but deliberate variations in method parameters (method’s reliability during normal usage) described by the robustness showed RSD% less than 4.6% measured by varying 3 different parameters. The validated method was successfully applied to simultaneously determine the concentration of the 3 new isoflavans having anti-inflammatory and antidiabetic activities. The results revealed that the validated method can be used for quality control of herbal preparations containing these or similar isoflavans that are marketed for the prevention of inflammation and as antidiabetics.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

scholarly journals Determination of donepezil in spiked rabbit plasma by high-performance liquid chromatography with fluorescence detection

2019 ◽  
Vol 6 (1) ◽  
pp. 181476
Author(s):  
Fardous A. Mohamed ◽  
Pakinaz Y. Khashaba ◽  
Reem Y. Shahin ◽  
Mohamed M. El-Wekil
Keyword(s):  
Fluorescence Detection ◽  
High Performance ◽  
Internal Standard ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
System Suitability ◽  
Peak Areas ◽  
Dispersive Liquid Liquid Microextraction ◽  
Bioanalytical Validation

The aim of this paper is to develop sensitive, accurate, reproducible and robust RP-HPLC with fluorescence detection for estimation of donepezil (DZ) in rabbit plasma using silodosin as the internal standard (IS). The prepared samples were quantified on reversed phase column Luna C 18(2) (150 × 4.6 mm i.d., 5 µm particle size) operated at room temperature using the mobile phase consisting of methanol: 0.1% acetic acid (50 : 50, v/v) at a flow rate of 1 ml min −1 . The method was fully validated according to bioanalytical validation guidelines of FDA in terms of system suitability, selectivity, sensitivity, precision and stability. It was found that the increase in peak areas followed the increase of DZ concentration in the range of 2.56–200.00 ng ml −1 with LOD of 0.85 ng ml −1 . The method was successfully applied for the determination of DZ in rabbit plasma using manual shaking dispersive liquid–liquid microextraction.

scholarly journals Determination of Neomycin and Oxytetracycline in the Presence of Their Impurities in Veterinary Dosage Forms by High-Performance Liquid Chromatography/Tandem Mass Spectrometry

2011 ◽  
Vol 94 (3) ◽  
pp. 750-757 ◽  
Author(s):  
Katarina Vučičevič-Prčetič ◽  
Robert Cservenák ◽  
Niko Radulović
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Dosage Forms ◽  
Analysis Time ◽  
Main Peak ◽  
Main Compound ◽  
Liquid Chromatography Tandem Mass

Abstract Two HPLC/MS/MS methods, one for determination of neomycin sulfate and the other for determination of oxytetracycline hydrochloride in the presence of their impurities, were developed and validated. Separations were achieved with gradient elution on a C18 column. All components were ionized by positive-ion electrospray and detected by multiple reaction monitoring. Calibration curves were linear, with correlation coefficients &gt;0.99. Precision of the methods was confirmed by RSD values of 0.34 and 0.71% for neomycin and oxytetracycline, respectively. Recovery values of 101.5 and 101.0%, respectively, indicated adequate accuracy. Analysis time for neomycin was 24 min, with the retention time of the main compound at 10.1 min; for oxytetracycline, the analysis time was 18 min, with the main peak at 9.95 min. Longer retention times than expected were a consequence of the necessity of chromatographic separation of isomers with the same ion transition. All impurities defined in the pharmacopoeias were determined and their identities confirmed. The methods were tested for QC of veterinary dosage forms (commercial powders and injections containing these antibiotics).

Liquid Chromatographic Determination of Lake Red C Amine and 2-Naphthol in D&C Red No. 8

1988 ◽  
Vol 71 (5) ◽  
pp. 1007-1011
Author(s):  
Alan L Scher ◽  
Robert J Calvey
Keyword(s):  
Chromatographic Determination ◽  
Gradient Elution ◽  
Column Method ◽  
Peak Areas ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Prediction Limits ◽  
Liquid Chromatographic ◽  
Cellulose Column

Abstract A method is described for the determination of the intermediates in D&C Red No. 8 by reverse-phase liquid chromatography (LC). The pigment is dissolved in boiling 95% ethanol-water (1 + 1) and then precipitated. The filtrate is chromatographed by gradient elution. Calibrations from peak areas at 254 nm for Lake Red C Amine sodium salt (LRCA-Na) and at 229 nm for 2-naphthol were linear, with prediction limits of 0.200 ± 0.006% and 0.200 ± 0.003%, respectively, for the maximum permitted levels. Calibration limits of determination were 0.01% for LRCA-Na and 0.006% for 2-naphthol. A 99% confidence level was used. Recoveries were 100.0-100.4% for LRCA-Na and 97.1-101.8% for 2-naphthol, each added at levels of 0.025-0.2%. Certified lots of D&C Red No. 8 that were analyzed by the LC method contained higher levels of LRCA-Na but the same levels of 2-naphthol when compared to results obtained previously by a cellulose column method, in which the pigment is not dissolved. The solubilities of D&C Red No. 8 in hot and room temperature solutions of 95% ethanol-water (1 + 1), water, and 95% ethanol were estimated.

High Pressure Liquid Chromatographic Determination of Putrefactive Amines in Foods

1983 ◽  
Vol 66 (4) ◽  
pp. 853-857 ◽  
Author(s):  
Julia Y Hui ◽  
Steve L Taylor
Keyword(s):  
High Pressure ◽  
Correlation Coefficients ◽  
Chromatographic Determination ◽  
Gradient Elution ◽  
High Pressure Liquid Chromatographic ◽  
Elution Time ◽  
Canned Tuna ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) procedure is described for determining the following putrefactive amines: histamine, tyramine, putrescine, cadaverine, tryptamine, and β-phenylethylamine. The amines were extracted from tuna or cheese with methanol. Futher cleanup was performed by sequential extractions with butanol and HC1. The acid extract was dried, and residues were derivatized with dansyl chloride. HPLC separations were performed on an Ultrasphere-ODS column at 33°C. A gradient elution program was used; the total elution time was less than 17 min. Linear standard curves with high correlation coefficients were obtained. The procedure allowed good recoveries of histamine, tyramine, putrescine, and cadaverine; recoveries of tryptamine and β-phenylethylamine were lower but constant. With this method, some swiss cheese samples were found to contain considerable amounts of histamine, tyramine, putrescine, cadaverine, and β-phenylethylamine. Canned tuna samples had very low levels of these amines. Since the presence of amines at high levels has been associated with tuna decomposition, this method may be useful in identifying decomposed fish.

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