Rapid Determination of Deoxynivalenol (Vomitoxin) by Liquid Chromatography Using Modified Romer Column Cleanup

1984 ◽  
Vol 67 (1) ◽  
pp. 52-54 ◽  
Author(s):  
Henry L Chang ◽  
Jonathan W Devries ◽  
Paul A Larson ◽  
Hasmukh H Patel
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Rapid Determination ◽  
Alumina Column ◽  
Relative Standard ◽  
Alumina Column Chromatography ◽  
Wheat Products ◽  
Liquid Chromatographic

Abstract A modification of the Romer method for determining deoxynivalenol (DON) provides rapid sample cleanup and includes liquid chromatographic (LC) quantitation. The method was evaluated using wheat, wheat flour, and other wheat products. The sample is extracted with acetonitrile–water (84 + 16), and an aliquot of the extract is subjected to activated charcoal–alumina column chromatography. The extract is then evaporated and diluted to volume with mobile phase, and DON is quantitated using liquid chromatography. The relative standard deviation based on duplicate samples is 6.07%. The detection limit is 30 ppb based on 2 x signal/noise ratio. Results by this method compared with the results obtained by the Scott GC method showed a correlation coefficient of 0.992 with a mean vomitoxin content of 779 ppb by this method and 716 ppb by the Scott method for 14 samples.

scholarly journals Determination of Patulin in Apple Juice by Liquid Chromatography

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Apple Juice ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Relative Standard ◽  
Precision Study

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

scholarly journals Determination of Olaquindox Residues in Swine Tissues by Liquid Chromatography

1987 ◽  
Vol 70 (4) ◽  
pp. 706-707 ◽  
Author(s):  
Tomoko Nagata ◽  
Masanobu Saeki
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Column Chromatography ◽  
Alumina Column ◽  
Ultraviolet Detection ◽  
Alumina Column Chromatography ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for determination of olaquindox residues in swine tissues. The drug is extracted from tissues with acetonitrile, and the extract is evaporated to dryness. This residue is cleaned up by alumina column chromatography. LC analysis is carried out on a Nucleosil C18 column, and olaquindox is quantitated by ultraviolet detection at 350 nm. The average recoveries of olaquindox added to tissues at levels of 0.2, 0.1, and 0.05 ppm were 74.0, 68.6, and 66.3%, respectively. The detection limit was 2 ng for olaquindox standard and 0.02 ppm in tissues.

Medium-pressure liquid chromatography of platinum metal ions on Spheron DEAE

1983 ◽  
Vol 48 (8) ◽  
pp. 2255-2262 ◽  
Author(s):  
František Vláčil ◽  
Ivan Vinš ◽  
Oldřich Malíček
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Metal Ions ◽  
Mobile Phase ◽  
Platinum Metal ◽  
Hydrochloric Acid Concentration ◽  
Chloride Medium ◽  
Relative Standard ◽  
Medium Pressure Liquid Chromatography

Spheron DEAE (modified macroreticular hydroxyethylmethacrylate-ethylenedimethacrylate copolymer) was used for chromatographic separation and determination of Rh(III), Pd(II), and Pt(IV) in chloride medium. The most suitable composition of the mobile phase was looked for by studying the influence of hydrochloric acid concentration on the capacity ratios of the metal ions mentioned and on their resolution, as well as the influence of different additions to the mobile phase on the decrease of the high Pt(IV) retention. Using the photometric (UV) detection, the linear dependence was found up to following concentrations: Rh 200 mg l-1, Pd 2 g l-1, Pt 500 mg l-1. The detection limit was 23 ng Rh, 62 ng Pd and 96 ng Pt in 7 μl sample injected.The reproducibility of the determination was (as relative standard deviation for n = 3) 1-4%, relative error 0.7-7%.

scholarly journals SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Retention Time ◽  
Analytical Method ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

Gas-Liquid Chromatographic Determination of Kepone Residues in Finfish, Shellfish, and Crustaceans

1978 ◽  
Vol 61 (4) ◽  
pp. 877-883
Author(s):  
Richard A Carver ◽  
Arnold P Borsetti ◽  
Laverne R Kamps
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Petroleum Ether ◽  
Ethyl Ether ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Finfish, shellfish, and crustacean samples are extracted with isopropanol and benzene; the extract is filtered and then concentrated. The extract, dissolved in hexane, is treated with oleum and extracted with aqueous alkali. The aqueous phase is acidified and extracted with petroleum ether-ethyl ether (1+1). The Kepone residue is determined by electron capture gas-liquid chromatography (GLC). Recoveries obtained by 8 laboratories from 15 species of finfish fortified at 0.02-0.23 ppm ranged from 37 to 107% with a mean ± relative standard deviation of 79.4±14.5%. For oysters fortified at 0.01- 0.10 ppm, recoveries range from 63 to 129% with a mean of 78.2 ±20.8%. For crustaceans fortified at 0.05—0.26 ppm, recoveries ranged from 52 to 110% with a mean of 78.8±16.4%. The approximate limits of quantitation for finfish and for shellfish and crustaceans are 0.02 and 0.05 ppm, respectively, under the GLC conditions used in this study.

Assay of Oxolinic Acid Residues in Salmon Muscle by Liquid Chromatography with Fluorescence Detection: Interlaboratory Study

1991 ◽  
Vol 74 (6) ◽  
pp. 906-909 ◽  
Author(s):  
Germain Carignan ◽  
Lyse Larocque ◽  
Sved Stephen ◽  
◽  
K Carrier ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Sample Preparation ◽  
Oxalic Acid ◽  
Fluorescence Detection ◽  
Oxolinic Acid ◽  
Fluorometric Detection ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A previously developed method that uses a simplified sample preparation and fluorometric detection of liquid chromatographic eluates for the determination of oxolinic acid in salmon muscle has been collaboratively studied. Five laboratories participated in the study to analyze, in quintuplicate, blank salmon muscle fortified at 10, 20, 50, and 100 μg/kg (ppb), and 2 incurred samples from salmon given feed with medicated oxolinic acid. The tissue, 2 g mixed with 2 g Na2S04, is extracted with ethyl acetate and centrifuged, and the solvent Is evaporated. The residue is partitioned in a mixture of hexane and 0.01 M oxalic acid, and the aqueous phase is chromatographed using fluorescence detection at 327 nm excitation and 369 nm emission. Mean recoveries ranged from 77.2 to 84.5% in spiked samples with reproducibility relative standard deviation (RSDR) ranging from 11.5 to 18.3%. Treated salmon were found to contain 8.71 and 53.8 μg/kg with RSDR of 18.6 and 16.7%, respectively. The corresponding repeatability relative standard deviations (RSDr) were 5.8-12.2%, and 7.7 and 6.2%. The method is recommended for regulatory purposes in Canada.

scholarly journals Simultaneous Determination of Rutin, Luteolin, Quercetin, and Betulinic Acid in the Extract ofDisporopsis pernyi(Hua) Diels by UPLC

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Yanqi Wang ◽  
Shuyi Li ◽  
Dandan Han ◽  
Kehan Meng ◽  
Miao Wang ◽  
...  
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Betulinic Acid ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Relative Standard ◽  
Quantitative Basis

Disporopsis pernyi(Hua) Diels, which belongs to genusDisporopsis, has been widely used for the treatment of abnormal sweating, chronic cough, and so forth. An ultra-performance liquid chromatography (UPLC) analysis was developed for the determination of rutin, luteolin, quercetin, and betulinic acid inDisporopsis pernyi(Hua) Diels roots. UPLC analysis was conducted by using a Shim-pack XR-ODS column with gradient elution with the mobile phase of acetonitrile and water containing 0.1% formic acid and with a flow rate of 0.2 mL/min, detected at 210, 254, and 280 nm. The method was precise, with relative standard deviation < 2.0%. The recoveries for the four components inDisporopsis pernyi(Hua) Diels were between 98.5 and 100.9%. The average contents of rutin, luteolin, quercetin, and betulinic acid in roots were 5.63, 2.51, 3.87, and 2.41 μg/g, respectively. The method was accurate and reproducible and it can provide a quantitative basis for quality control ofDisporopsis pernyi(Hua) Diels.

Liquid Chromatographic Determination of the Herbicide Isoxaben and Its Soil Metabolite in Soil and Soil-Turf Samples

1990 ◽  
Vol 73 (2) ◽  
pp. 287-289 ◽  
Author(s):  
Bonnie S Rutherford
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Column Chromatography ◽  
Chromatographic Determination ◽  
Alumina Column ◽  
Alumina Column Chromatography ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method Is described for the determination of residues of isoxaben and its principal soil metabolite In soil and soil-turf samples. Both compounds are extracted from samples by refluxing with methanol-water. An aliquot of the extract Is partitioned Into dichloromethane and purified by alumina column chromatography. Separate fractions containing isoxaben and metabolite are collected and subjected to liquid chromatography at conditions that are optimized for each compound. The detection limit for both compounds is 0.005 ppm. Residue identities are confirmed by chromatography on a different LC system.

Liquid Chromatographic Assay of Dimetridazole, Ipronidazole, and Ronidazole in Feeds and Premixes

1992 ◽  
Vol 75 (4) ◽  
pp. 663-666 ◽  
Author(s):  
B Tollomelli ◽  
R Laffi ◽  
S Rossato ◽  
G Colpo
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Rapid Method ◽  
Reversed Phase ◽  
Uv Detection ◽  
Reversed Phase Liquid Chromatography ◽  
Alumina Column ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A rapid method has been developed for the determination of dimetridazole (DMZ), ipronidazole (IPZ), and ronidazole (RNZ) in turkey feeds, swine feeds, and premix. The compounds are extracted from samples with warm methanol, the extract is purified over a short alumina column, and an aliquot of the eluate is analyzed by reversed-phase liquid chromatography and UV detection at 309 nm. Alumina cleanup of premixes is not essential, although the resulting chromatograms are cleaner. Recoveries of DMZ from feed formulations ranged from 97 to 103% at the 10.0,50.0, and 100.0 ppm levels, with a standard deviation (SD) of 0.62-3.2%. Recoveries of IPZ ranged from 94.4 to 101.2% at the 5.0,50.0, and 100.0 ppm levels (SD, 0.42-4.4%). RNZ recoveries ranged from 95 to 100.7% at the 6.0,60.0, and 120.0 ppm levels (SD, 1.2-5.33%).

Liquid Chromatographic Determination of the Anticoccidial Drug Halofuginone Hydrobromide in Eggs

1995 ◽  
Vol 78 (1) ◽  
pp. 37-40 ◽  
Author(s):  
David C Holland ◽  
Robert K Munns ◽  
Jose E Roybal ◽  
Jeffrey A Hurlbut ◽  
Austin R Long
Keyword(s):  
Standard Deviation ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Chromatographic Determination ◽  
Free Base ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for the determination of 5-100 ppb halofuginone hydrobromide (HFG) in eggs. HFG as the free base is extracted from eggs with ethyl acetate. The extract is cleaned up on an acidic Celite 545 column. A Waters C18 column is used for LC separation with UV determination at 243 nm. The isocratic mobile phase is a mixture of water-acetonitrile-ammonium acetate buffer (12 + 5 + 3) and acetic acid. The interassay average recovery from eggs was 90.4%, with a standard deviation of 5.11 and a relative standard deviation of 5.65%.

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