Fluorometric Method for Determination of 1,2-Unsaturated Aldehydes in Autooxidized Lipids with 2,4-Diaminotoluene

1990 ◽  
Vol 73 (4) ◽  
pp. 590-594
Author(s):  
Teruhisa Hirayama ◽  
Shinji Miura ◽  
Mariko Araki ◽  
Yoshiko Takeo ◽  
Tetsushi Watanabe
Keyword(s):  
Methyl Oleate ◽  
Acidic Condition ◽  
Emission Wavelength ◽  
Excitation Wavelength ◽  
Fluorometric Method ◽  
Unsaturated Aldehydes ◽  
Liquid Chromatographic

Abstract A simple fluorometric method has been developed to determine 1,2-unsaturated aldehydes in autooxidized lipids. 1,2- Unsaturated aldehydes were allowed to react with 2,4-diamlnotoluene in acidic condition and the products, 7-amlno-6- methylqulnoline derivatives, were determined by a fluorometric procedure at 394 nm (excitation wavelength) and 494 nm (emission wavelength). Finally, 1902.9, 1738.8, and 2149.2 μg/g of 1,2-unsaturated aldehydes as 2-propenal were detected in 20-h autooxidized methyl oleate, methyl llnoleate, and methyl llnolenate, which contained 98.5, 223.2, and 355.6 μg/g, respectively, of thlobarblturlc acid reactive substances as malondialdehyde. In a preliminary liquid chromatographic LC determination of 2-propenal In autooxidized lipids, 29, 20, and 57 μg/g, respectively, of 2- propenal were detected In 20-h autooxidized methyl oleate, methyl llnoleate and methyl llnolenate. The 2-propenal can be detected as 7-amlno-6-methylqulnoline by using LC-fluorometrlc procedure at levels of 100 pg.

Sensitive Fluorometric Method for Determination of Quercetin in Plasma or Urine

1973 ◽  
Vol 19 (1) ◽  
pp. 36-37 ◽  
Author(s):  
R Gugler ◽  
H J Dengler
Keyword(s):  
Emission Wavelength ◽  
Flavonoid Compound ◽  
Excitation Wavelength ◽  
Fluorometric Method

Abstract A fluorometric method is described for determining quercetin, a flavonoid compound, in plasma and urine. It is based on the formation of the highly fluorescent quercetin-tetraphenyldiboroxide complex. The excitation wavelength used is 445 nm, the emission wavelength 500 nm.

Fluorometric estimation of triglycerides in serum by a modification of the method of Bucolo and David.

1977 ◽  
Vol 23 (2) ◽  
pp. 286-288 ◽  
Author(s):  
E B Rietz ◽  
G G Guilbault
Keyword(s):  
Blood Serum ◽  
Spectrophotometric Method ◽  
Serum Triglyceride ◽  
Excitation Wavelength ◽  
Free Glycerol ◽  
Fluorometric Method ◽  
Nadh Fluorescence ◽  
Instrument Response ◽  
Serum Triglyceride Concentration

Abstract An enzymic, flurometric method is described for determination of triglycerides (and glycerol) in blood serum, a modification of the method of Bucolo and David [Clin. Chem. 19, 476 (1973)]. Commercially available reagent kits are used. The rate of disappearance of NADH fluorescence at 460 nm (excitation wavelength, 365 nm) is monitored and related to serum triglyceride concentration, corrected for the content of free glycerol. We compared the results obtained fluorometrically to the ultraviolet spectrophotometric Boehringer Neutral Fat method used at Gentofte Hospital, Copenhagen. Instrument response and concentration were linearly related in the range 0.27 to 2.7 mmol of triglycerides per liter of serum with the fluorometric method. The CV was 0.9% for the fluorometric method, 3.7% for the spectrophotometric procedure. The fluorometric method requires less reagents, time, and calculations than does the spectrophotometric method.

Rapid Fluorometric Determination of Benzo(a)pyrene in Foods

1982 ◽  
Vol 45 (2) ◽  
pp. 139-142 ◽  
Author(s):  
YASUHIDE TONOGAI ◽  
SHUNJIRO OGAWA ◽  
MASATAKE TOYODA ◽  
YOSHIO ITO ◽  
MASAHIRO IWAIDA
Keyword(s):  
Detection Limit ◽  
Peak Height ◽  
Excitation Wavelength ◽  
Activated Alumina ◽  
Fluorometric Method ◽  
Fluorometric Determination ◽  
Standard Curve ◽  
Layer Chromatography ◽  
Entire Procedure

A simple and rapid fluorometric method for determining benzo (a) pyrene in foods was developed. Benzo (a) pyrene is extracted from foods with n-hexane:ether mixture (4:1), purified through a column of activated alumina and determined fluorometrically. An excitation wavelength of 295 nm and emission wavelength of 403 nm were used for calculating concentrations of benzo (a) pyrene. The peak height at 403 nm and baseline between 392 and 418 nm were employed to derive a standard curve for quantitating benzo (a) pyrene. A calibration curve for between 0.04 – 4 ng/ml of benzo (a) pyrene was used. Recoveries of benzo (a) pyrene from 14 kinds of food spiked at levels of 20 and 2ppb were within the range of 79.5 – 93.8% and 50.0 – 80.6%, respectively. The entire procedure takes only one hour with the detection limit being 0.1 ppb. Benzo (a) pyrene detected was reconfirmed by thin-layer chromatography.

scholarly journals Determination of Decoquinate in Animal Feeds by Liquid Chromatography: Collaborative Study

2008 ◽  
Vol 91 (4) ◽  
pp. 685-693 ◽  
Author(s):  
Anivis A Sanchez ◽  
Harold M Campbell ◽  
M S Ahmed ◽  
K Albert ◽  
C Applegate ◽  
...  
Keyword(s):  
Collaborative Study ◽  
The United States ◽  
Reversed Phase ◽  
Excitation Wavelength ◽  
Mechanical Agitation ◽  
Trace Level ◽  
Animal Feeds ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract The performance characteristics of a liquid chromatographic (LC) method for the analysis of decoquinate (DEC) in supplements, premixes, and complete animal feeds at medicating and trace levels were collaboratively studied. DEC is extracted from ground feed samples with 1 calcium chloridemethanol solution using mechanical agitation for 90 min. After centrifugation for 5 min and dilution (if necessary), an aliquot of the extract is diluted with water. The diluted extracts are filtered and analyzed by reversed-phase LC with fluorescence detection. Suspect positive trace-level samples are confirmed by using an alternate excitation wavelength. Fourteen test samples of medicated feeds, supplement, and medicated premix, along with 8 test samples for trace-level analysis, were sent to 13 collaborators (one in Canada, 4 in Europe, and 8 in the United States). Test samples were analyzed as blind duplicates. Acceptable results were received from 12 laboratories for the medicated test samples and from 13 laboratories for the trace-level samples. Repeatability relative standard deviation estimates ranged from 1.3 to 5.6. Reproducibility relative standard deviations estimates ranged from 2.8 to 6.1, and HorRat values ranged from 0.22 to 0.74.

Evaluation of a direct fluorometric method for determination of serum retinol.

1986 ◽  
Vol 32 (5) ◽  
pp. 867-869 ◽  
Author(s):  
W J Driskell ◽  
J S Hewett ◽  
M M Bashor
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Retinol Binding Protein ◽  
Serum Retinol ◽  
Fluorometric Method ◽  
Fluorescence Excitation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract We evaluated the usefulness of a fluorometric method for determining serum retinol (Futterman et al., Invest Ophthalmol Vis Sci 1975;14:125-30) in which fluorescence (excitation 335 nm; emission 460 nm) of retinol is directly measured in unextracted, diluted serum. Using serum from 466 individual donors, we compared values so obtained with those by a "high-performance" liquid-chromatographic method. The correlation coefficient (r) was 0.74. When we compared fluorometric retinol values with retinol-binding protein values for the 466 samples, r was 0.71. About 1% of the 466 samples had markedly higher values by fluorometry than by chromatography, the result of positive interferences. For two serum pools, we obtained CVs of 1.58% (n = 57) and 1.79% (n = 57) in long-term precision studies lasting 60 days. Although the fluorometric method of Futterman et al. has not been widely adopted, we find that it is simple to perform and that results compare favorably with the chromatographic method in precision and accuracy. It is unique among commonly used serum retinol methods in that the serum need not be extracted with organic solvents.

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.

Determination of Ergotamine Tartrate in Tablets by Liquid Chromatography with Fluorescence Detection

1987 ◽  
Vol 70 (3) ◽  
pp. 538-540
Author(s):  
Ugo R Cieri
Keyword(s):  
Mobile Phase ◽  
Small Volume ◽  
Excitation Wavelength ◽  
Reverse Phase ◽  
Volumetric Flask ◽  
Relative Standard ◽  
Liquid Chromatographic ◽  
Ergotamine Tartrate ◽  
Phase Column

Abstract A method is presented for the liquid chromatographic (LC) determination of ergotamine tartrate in tablets that is applicable even in the presence of other ingredients such as phenobarbital, belladonna alkaloids, and caffeine. The sample is transferred to a volumetric flask, a small volume of formic acid is added to dissolve and stabilize the ergotamine, and the solution is diluted to volume with methanol. The solution is mixed and filtered through paper. The LC system consists of a Rheodyne injector fitted with a 20 μL loop and a C,18 reverse phase column; the mobile phase is acetonitrile-water-triethylamine (700 + 300 + 0.5). Ergotamine tartrate is determined fluorometrically at an excitation wavelength of 250 nm and an emission wavelength of 430 nm. Recovery studies were conducted at the 0.3 and 1.0 mg levels. Average recoveries were 99.6 and 100.8%, respectively; relative standard deviations (RSDs) were 1.08 and 2.21%, respectively. Some commercial preparations containing ergotamine tartrate in combination with other ingredients were also analyzed. The RSDs for 5 determinations of each of 2 ground composites were 0.09 and 0.34%.

Gas-Liquid Chromatographic Determination of Selenium in Biological Materials, Using 4-Bromo- and 4-Chloro-1,2-Diaminobenzene as Derivatizing Reagents

1978 ◽  
Vol 61 (4) ◽  
pp. 923-926
Author(s):  
Brian M Bycroft ◽  
Donald E Clegg
Keyword(s):  
Atomic Absorption ◽  
Fish Meal ◽  
Chromatographic Determination ◽  
Biological Materials ◽  
Meal Sample ◽  
Fluorometric Method ◽  
Chloro Derivative ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is described for the gas-liquid chromatographic determination of traces of selenium in marine biological materials. The method is based on the reaction of Se(IV) with bromo- and chloro-substituted 1,2-diaminobenzenes. The benzoselenadiazoles so formed are sensitive to electron capture detection. The sample is digested in a nitric-perchloric acid mixture and selenium is reduced to the IV oxidation state. Different aliquots of the digest solution are reacted with either 4-bromo- or 4-chloro-l,2-diaminobenzene to quantitatively form the corresponding 2,1,3-benzoseIenadiazole. Recovery of added selenite to a fish meal sample was 95% for the bromo derivative and 101% for the chloro derivative. Different portions of a well mixed fish meal sample were analyzed in independent laboratories by the fluorometric method and by atomic absorption spectrophotometry (hydride generation). The following mean values (μg/g) were found: present method 1.89, fluorometric method 1.91, atomic absorption method 2.1. The lower limit of detection for the method described was 13 ng, using the bromo derivative, and 27 ng, using the chloro derivative.

Simple Fluorometric Method for Estimating Practolol [1-(4-Aminophenoxy)-3-isopropylaminopropan-2-ol] in Blood and Urine

1972 ◽  
Vol 18 (4) ◽  
pp. 363-365 ◽  
Author(s):  
Gunter Bodem ◽  
Charles A Chidsey
Keyword(s):  
Receptor Antagonist ◽  
Adrenergic Receptor ◽  
Weak Acid ◽  
Emission Wavelength ◽  
Excitation Wavelength ◽  
Fluorometric Method ◽  
Beta Adrenergic Receptor ◽  
Beta Adrenergic

Abstract A fluorometric method has been devised for determining practolol [1-(4-aminophenoxy)-3-isopropylaminopropan-2-ol], a new beta-adrenergic receptor antagonist, in blood and urine. The conjugate of deacetylated practolol with nitrosonaphthol is highly fluorescent in weak acid. The excitation wavelength used is 460 nm, the emission wavelength 550 nm.

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.

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