scholarly journals Analysis of Fumonisin Bi and Its Hydrolysis Product in Tortillas

1998 ◽  
Vol 81 (4) ◽  
pp. 737-740 ◽  
Author(s):  
Michael E Stack

Abstract Fumonisins are toxic metabolites of Fusarium moniliforme, a fungus that occurs widely in corn. Fumonisins cause leukoencephalomalacia in horses and pulmonary edema in swine and have been suggested as a possible cause of an increased incidence of neural tube defects among people living along the Texas-Mexico border. As part of an effort to determine levels of fumonisins in human food, a liquid chromatographic (LC) method was devised for determining fumonisin Bi (FB1) and the total hydrolysis product of FB1 (HB1) in tortillas. The method uses acetonitrile-0.1M phosphate buffer (pH 3; 1 +1) extraction, solidphase C18 cleanup, ophthalaldehyde and 2-mercaptoethanol derivatization, and reversed-phase LC. Average recoveries from tortillas spiked with FB1 and HB1 at 250, 500, and 1000 ng/g were 86.5℅ for FB1 and 82.6℅ for HB1. Tortillas (54) and masa (8) from the Texas-Mexico border were analyzed for FB1 and HB1. Average amounts of FB1 and HB1 in tortillas were 187 and 82 ng/g, respectively. Average amounts of FB1 and HB1 in masas were 262 and 64 ng/g, respectively. The results show that fumonisin B1 and its hydrolysis product are present in tortillas consumed by a population experiencing an increased incidence of neural tube defects.

1997 ◽  
Vol 80 (5) ◽  
pp. 1111-1116 ◽  
Author(s):  
Ronald J Scholefield ◽  
Karen S Slaght ◽  
John L Allen

Abstract Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys {Petromyzon marinug) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)-Nmethylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a Cis column, amobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).


1995 ◽  
Vol 78 (2) ◽  
pp. 289-293
Author(s):  
Hafez Abdel-Kader ◽  
Myriam M Kobylkevich ◽  
Larry S Wigman ◽  
Govind K Menon

Abstract A liquid chromatographic (LC) method was developed for the determination of ardacin in bulk chemical (78 to 100%, w/w anhydrous) and premix formulations (3.3 to 26.4%, w/w). The method is based on reversed-phase LC resolution of ardacin components and detection by UV absorbance at 220 nm. Ardacin has 10 components, and each component can be quantitated separately. Total ardacin is determined by summing the areas of the 10 component peaks. Calculations are performed using an external standard approach. The method is linear for ardacin at 50 to 150 μ/mL. The method accuracy for a typical bulk chemical is ± 1.5%, w/w (relative standard deviation [RSD], 1.6%), and recovery from a typical pilot scale premix is 99.9% (RSD, 3.4%). The method is useful for monitoring stability during storage.


1996 ◽  
Vol 79 (2) ◽  
pp. 451-455 ◽  
Author(s):  
Allan R Brause ◽  
Mary W Trucksess ◽  
Frederick S Thomas ◽  
Samuel W Page ◽  
J Burke ◽  
...  

Abstract An AOAC International-International Union of Pure and Applied Chemistry-International Fruit Juice Union (AOAC-IUPAC-IFJU) collaborative study was conducted to evaluate a liquid chromatographic (LC) procedure for determination of patulin in apple juice. Patulin is a mold metabolite found naturally in rotting apples. Patulin is extracted with ethyl acetate, treated with sodium carbonate solution, and determined by reversed-phase LC with UV detection at 254 or 276 nm. Water, water-tetrahydrofuran, or water-acetonitrile was used as mobile phase. Levels determined in spiked test samples were 20, 50,100, and 200 μg/L. A test sample naturally contaminated at 31 μg/L was also included. Twenty-two collaborators in 10 countries analyzed 12 test samples of apple juice. Recoveries averaged 96%, with a range of 91-108%. Repeatability relative standard deviations (RSDr) ranged from 10.9 to 53.8%. The reproducibility relative standard deviation (RSDR) ranged from 15.1 to 68.8%. The LC method for determination of patulin in apple juice has been adopted first action by AOAC INTERNATIONAL.


1999 ◽  
Vol 149 (12) ◽  
pp. 1119-1127 ◽  
Author(s):  
K. A. Hendricks ◽  
J. S. Simpson ◽  
R. D. Larsen

2003 ◽  
Vol 86 (3) ◽  
pp. 510-514 ◽  
Author(s):  
Jeffery M van de Riet ◽  
Ross A Potter ◽  
Melissa Christie-Fougere ◽  
B Garth Burns

Abstract A liquid chromatographic (LC)/mass spectrometric (MS) method was developed for determining the residues of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in a number of aquatic species. The phenicols are extracted with acetone, the extracts are partitioned with dichloromethane, the aqueous layer is removed, and the organic layer is evaporated to dryness. The residue is dissolved in dilute acid and defatted with hexane, and the aqueous layer is prepared for analysis by LC. The phenicols are determined by reversed-phase LC by using a Hypersil C18-BD column with a water–acetonitrile gradient and MS detection using selectedion recording. Calibration curves were linear for all analytes between 0.015 and 0.425 ng injected. The relative standard deviations for measurements by the proposed method were <10% for all of the analytes studied, with re-coveries ranging from 71% for florfenicol amine to 107% for florfenicol in salmon tissue spiked at the 2 ng/g level. Detection limits of 0.1 ng/g for florfenicol and chloramphenicol, 0.3 ng/g for thiamphenicol, and 1.0 ng/g for florfenicol amine are easily obtainable. The operational errors, interferences, and recoveries for spiked samples compare favorably with those obtained by established LC methodology. The proposed method is simple, rapid, and specific for monitoring residues of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in a number of aquatic species.


2006 ◽  
Vol 2006 (Suppl4) ◽  
pp. 67-72 ◽  
Author(s):  
K.A. Voss ◽  
R.T. Riley ◽  
J.B. Gelineau-van Waes

1994 ◽  
Vol 77 (6) ◽  
pp. 1341-1346
Author(s):  
Hafez Abdel-Kader ◽  
Sylvia V Fagan ◽  
Govtnd K Menon ◽  
Larry S Wigman ◽  
Frederic Chapin

Abstract A rapid and sensitive 2-peak liquid chromatographic (LC) method is described for extracting and quantitating ardacin in premix, supplement, and animal feed formulations. Ardacin is extracted from the formulations and analyzed after dilution or cleanup by reversed-phase LC with UV detection at 220 nm. The method correlates well with a more information-rich gradient multipeak LC method. Recoveries for premix formulations ranged from 96.8% (relative standard deviation [RSD], 0.8%) to 103.7% (RSD, 1.3%) for laboratory samples spiked at levels ranging from 1.6 to 39.6% ardacin. Recoveries for protein supplement mash formulations ranged from 98.7% of claim (RSD, 4.1%) to 106.0% of claim (RSD, 7.7%) at ardacin levels ranging from 37.5 to 600 mg/lb. Recoveries for cattle feed ranged from 90.0% of claim (RSD, 11.9%) to 105.6% of claim (RSD, 2.7%) at ardacin levels ranging from 4 to 30 g/ton.


Teratology ◽  
2002 ◽  
Vol 66 (4) ◽  
pp. 169-176 ◽  
Author(s):  
T.W. Sadler ◽  
Alfred H. Merrill ◽  
Victoria L. Stevens ◽  
M. Cameron Sullards ◽  
Elaine Wang ◽  
...  

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