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.

Sorption of Se (IV) from aqueous solutions with subsequent determination by X-ray fluorescence analysis

2020 ◽  
Vol 86 (10) ◽  
pp. 5-9
Author(s):  
D. G. Filatova ◽  
A. A. Arkhipenko ◽  
M. A. Statkus ◽  
V. V. Es’kina ◽  
V. B. Baranovskaya ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
Fluorescence Analysis ◽  
Standard Samples ◽  
Phase Contact Time ◽  
Sorbent Phase ◽  
X Ray ◽  
Fundamental Parameters ◽  
Inductively Coupled ◽  
Subsequent Determination

An approach to sorptive separation of Se (IV) from solutions on a novel S,N-containing sorbent with subsequent determination of the analyte in the sorbent phase by micro-x-ray fluorescence method is presented. The sorbent copolymethylenesulfide-N-alkyl-methylenamine (CMA) was synthesized using «snake in the cage» procedure and proven to be stable in acid solutions. Conditions for quantitative extraction of Se (IV) were determined: sorption in 5 M HCl or 0.05 M HNO3 solutions when heated to 60°C, phase contact time being 1 h. The residual selenium content in the solution was determined by inductively coupled plasma mass spectrometry (ICP-MS) using 82Se isotope. The absence of selenium losses is proved and the mechanism of sorption interaction under specified conditions is proposed. The method of micro-x-ray fluorescence analysis (micro-RFA) with mapping revealed a uniform distribution of selenium on the sorbent surface. The possibility of determining selenium in the sorbent phase by micro-RFA is shown. When comparing the obtained results with the results of calculations by the method of fundamental parameters, it is shown the necessity of using standard samples of sorbates to obtain correct results of RFA determination of selenium in the sorbent phase.

ESTIMATION OF TADALAFIL IN HUMAN PLASMA BY SPECTROFLUOROPHOTOMETRY

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (06) ◽  
pp. 60-63
Author(s):  
Sadhana Rajput ◽  
◽  
Samir Patel ◽  
Keyword(s):  
Human Plasma ◽  
Fluorescence Spectrum ◽  
Drug Monitoring ◽  
Limit Of Detection ◽  
Wave Length ◽  
Excitation Wavelength ◽  
Limit Of Quantification ◽  
Pharmacokinetic Investigation ◽  
Satisfactory Recovery

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.

scholarly journals ELIMINASI GANGGUAN MATRIKS DALAM ANALISIS MERKURI HG SEBAGAI SENYAWA KOMPLEKS THIO MICHLER’S KETON SECARA SPEKTROFOTOMETRI

2016 ◽  
Vol 11 (1) ◽  
Author(s):  
Sukib Sukib ◽  
Muti'ah Muti'ah
Keyword(s):  
Solvent Extraction ◽  
River Water ◽  
Complex Compound ◽  
Limit Of Detection ◽  
Standard Addition ◽  
Analysis Method ◽  
Addition Method ◽  
Matrix Interferences ◽  
Mercury Analysis

Abstrak. Telah dilakukan penelitian tentang penyusunan metode analisis merkuri melalui pembentukan senyawa kompleks dengan 4,4'-Bis(dimethylamino)thio-benzophenone TMK. Senyawa kompleks tersebut berwarna biru kehijauan yang dapat dideteksi dengan  spektrofoto-meter pada kondisi: lmax 574 nm;  pH 3; konsentrasi TMK 0,0002 M, dan waktu tunggu selama 4–10 menit. perbandingan volume pereaksi: Hg(II), bufer pH 3, TMK 0,002 M, H2O bebas ion adalah 1:1:1:7. Dari hasil penelitian menunjukkan bahwa metode ini telah memenuhi validitas, yaitu: linieritas 0,05–2,0 mg/L, limit deteksi 0,008 mg/L, dan % recovery antara 98% – 102%. Gangguan matriks akibat adanya ion–ion Au(III), Ag(I), Pd(II), Cu(II), Co(II), dan Fe(II) dapat dieliminasi dengan metode ekstraksi pelarut dan adisi standar. Metode adisi standar terbukti mampu memberikan data hasil pengukuran yang dapat dipercaya pada a 5%, yaitu untuk sampel buatan sebesar (0,053 ± 0,001) mg/L, air sungai (0,034 ± 0,004) mg/L, dan sedimen sebesar (4,172 ± 0,050) mg/kg. Dari hasil penelitian ini dapat disimpulkan bahwa metode ekstraksi pelarut dan adisi standar mampu mengeliminasi gangguan matriks pada analisis merkuri sebagai kompleks Hg-TMK secara spektrofotometriKata kunci: Metode analisis merkuri, Thio Michler’s keton, eliminasi, gangguan matriks  Abstract. A research  of analysis method for determination of mercury through formation of complex with 4,4'-bis(dimethylamino)thiobenzophenone TMK has been conducted. The green blue complex compound can be detected with spectrophoto-meter in conditions: lmax 574 nm, buffer acetate pH 3, concentration of TMK 0,0002 M, and the absorbance of complex remains stable for 4–10 minutes. The formula of reagents volume for: Hg(II): buffer acetate pH 3: TMK 0,002 M : de-ionized water is 1:1:1:7. This method is valid, with parameters such as linearity 0.05–2.00 mg/L, limit of detection 0.008 mg/L, and recovery in the range 98%-102%. Matrix interferences that are caused by Au(III), Ag(I), Pd(II), Cu(II), Co(II), and Fe(III) ions can be eliminated with solvent extraction and standard addition methods. Standard addition method is able to give data of trusty measurement result at a 5%, that is for synthesis sample as (0.053 ±  0.001) mg/L, river water (0.034 ± 0.004) mg/L, and for sediment (4.172 ± 0.050) mg/kg. From the result of this research, it can be concluded that solvent extraction and standard addition methods are able to eliminated matrix interferences in mercury analysis as Hg-TMK complex spectrophotometrically Key waords: mercury analysis method, Thio Michler’s ketone, elimination, matrix interferences

Liquid Chromatographic Determination of Zearalenone and Zearalenol in Animal Feeds and Grains, Using Fluorescence Detection

1986 ◽  
Vol 69 (5) ◽  
pp. 894-898 ◽  
Author(s):  
Renee W Bagneris ◽  
Jean A Gaul ◽  
George M Ware
Keyword(s):  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Excitation Wavelength ◽  
Animal Feeds ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Sorghum Silage ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was developed for the determination of zearalenone and zearalenol in grains and mixed animal feeds. Samples are extracted with chloroform and purified by a baseacid liquid-liquid partition. Zearalenone and zearalenol are separated by reverse phase LC and determined by fluorescence detection, excitation wavelength 236 nm with a 418 nm cutoff filter. The method was applied to the determination of zearalenone and zearalenol in 395 survey samples of corn, oats, barley, sorghum, silage, and finished feeds. The limit of detection is 10 ng/g for both toxins. The range of naturally occurring toxins found was 10-4000 ng/g. Average recoveries were 84% for zearalenone and 69% for zearalenol. Coefficients of variation were 24.6% for zearalenone and 30.8% for zearalenol for crop year 1980, and 28.3% for zearalenone and 22.0% for zearalenol for crop year 1981.

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 Kinetic- spectrophotometric Method for the Determination of Naringenin in Pure and Supplements Formulations

2019 ◽  
Vol 16 (3) ◽  
pp. 0595
Author(s):  
ALmashhadani Et al.
Keyword(s):  
Prussian Blue ◽  
Correlation Coefficient ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Fixed Time ◽  
Calibration Graph ◽  
Maximum Absorbance ◽  
Kinetic Spectrophotometric

          Simple, cheap, sensitive, and accurate kinetic- spectrophotometric method has been developed for the determination of naringenin in pure and supplements formulations. The method is based on the formation of Prussian blue. The product dye exhibits a maximum absorbance at 707 nm. The calibration graph of naringenin was linear over the range 0.3 to 10 µg ml-1 for the fixed time method (at 15 min) with a correlation coefficient (r) and percentage linearity (r2%) were of 0.9995 and 99.90 %, respectively, while the limit of detection LOD was 0.041 µg ml-1. The method was successfully applied for the determination of naringenin in supplements with satisfactory results.

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).

X-Ray Fluorescence Analysis of Portland Cement Through the Use of Experimentally Determined Correction Factors

1973 ◽  
Vol 17 ◽  
pp. 214-224
Author(s):  
C. H. Anderson ◽  
J. E. Mander ◽  
J. W. Leitner
Keyword(s):  
Portland Cement ◽  
Fluorescence Analysis ◽  
Reference Standards ◽  
Primary Radiation ◽  
Correction Factors ◽  
Standard Samples ◽  
Cement Sample ◽  
Average Deviation ◽  
X Ray

AbstractCorrection factors, termed α-factors, similar to those defined by LaChance and Traill have been generated by the addition of variable, known amounts of individual oxides, or other compounds, to a base cement sample and measuring the x-ray intensities of the elements of interest. The effects of all common constituents of cement on the determination of CaO, SiO2 and Al2O3 were found. Factors for rhodium and chromium primary radiation were determined and, in general, showed small but significant differences. The factors for rhodium at 50kV and 30kV were substantia11y identical. The correction factors were tested through the use of the NBS 1011- 1016 cements as reference standards to analyze the new proposed NBS cement series. The correction factors not only furnished improved calibration curves, but also allowed the determination of CaO, Al2O3 and SiO2 with an average deviation of less than 0.2% (absolute) from the provisional values furnished with the standard samples.

scholarly journals Determination of Pyrimethamine in Animal Tissue and Egg by Liquid Chromatography with Fluorescence Detection

2001 ◽  
Vol 84 (4) ◽  
pp. 1031-1034 ◽  
Author(s):  
Shozo Horii ◽  
Masatoshi Nishi ◽  
Naoto Oku ◽  
Hiroyuki Miyakawa ◽  
Masakatsu Tezuka
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Animal Tissue ◽  
Excitation Wavelength ◽  
Chicken Muscle ◽  
Standard Calibration ◽  
Liquid Chromatographic ◽  
Fluorescent Derivative

Abstract A sensitive and selective liquid chromatographic (LC) assay was developed to determine the concentration of pyrimethamine in animal tissue and egg by fluorescent derivative. Animal samples were extracted with acetonitrile, centrifuged, and purified by hexane. Fluorescent derivatization was performed by reacting pyrimethamine with chloroacetaldehyde and subjected to LC with fluorescence detection (excitation wavelength 300 nm, emission wavelength 420 nm). The limit of detection was 10 ng/g (10 ppb) and the standard calibration curve was linear in the range of 1–100 ppb (0.01–1 ng/10 μL). Recoveries from samples fortified at levels of 0.1 and 1 ppm (μg/g) were 61.0–77.4 and 65.5–81.2%, respectively. The method was applied to the monitoring of marketed samples. Pyrimethamine was not determined in any of the 70 samples: 20 swine muscle; 20 chicken muscle; 10 chicken liver; and 20 egg.

scholarly journals SPECTROPHOTOMETRIC METHODS FOR THE QUANTIFICATION OF CARISOPRODOL USING FERRIC CHLORIDE, O-PHENANTHROLINE, AND P-NITROANILINE, SODIUM NITRITE AS ANALYTICAL REAGENTS

2019 ◽  
pp. 384-390
Author(s):  
MURALI D ◽  
PURNA CHANDRA RAO G
Keyword(s):  
Correlation Coefficient ◽  
Ferric Chloride ◽  
Sodium Nitrite ◽  
Sodium Nitrate ◽  
Limit Of Detection ◽  
Colored Complex ◽  
Spectrophotometric Methods ◽  
Analytical Reagents ◽  
Optimized Conditions

Objective: The present study represents the development of two spectrophotometric methods for the determination of carisoprodol (CCP) in pure and formulations using ferric chloride, o-phenanthroline, and p-nitroaniline (PNA), sodium nitrate as analytical reagents. Methods: The proposed spectrophotometric methods were developed based on oxidation of Fe3+ by CCP, and then, the resultant product was reacted with o-phenanthroline in acidic condition forms an orange-colored complex and diazotization of PNA followed by coupling with CCP in an alkaline medium forms yellow-colored complex. Results: Under the optimized conditions, the absorbance of CCP concentration obeyed the Beer’s law in the ranges of 10–60 μg/mL with good correlation coefficient values of 0.9992 and 0.9990 with the limit of detection values of 1.286 and 2.408 μg/mL, respectively. Conclusion: The proposed methods were successfully applied for the determination of CCP in pure and in their formulations.

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