High Pressure Liquid Chromatographic Determination of Ochratoxin A and Zearalenone in Cereals

1979 ◽  
Vol 62 (5) ◽  
pp. 1165-1168
Author(s):  
Egon Josefsson ◽  
Tord Möller
Keyword(s):  
High Pressure ◽  
Ochratoxin A ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Ultraviolet Detector ◽  
In Series ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method has been developed for determining ochratoxin A and zearalenone in cereals. The sample is extracted with phosphoric acid and chloroform. The extract is cleaned by washing on a silica gel column with cyclohexane-ethylene dichlorideethyl ether. After eluting zearalenone with chloroform, ochratoxin A is eluted with chloroformformic acid. Zearalenone is extracted into alkaline solution, washed with chloroform, the pH is adjusted, and the zearalenone is extracted back into chloroform. Ochratoxin A is purified by chromatography on aqueous sodium bicarbonate-Celite. The mycotoxins are determined by using a liquid chromatograph with 2 columns in series packed with Spherisorb ODS 10 μm and 5 μm, respectively. Ochratoxin A is detected with a spectrophotofluorometer, coupled in series with an ultraviolet detector for estimation of zearalenone. Detection limits are 1-5 μg/kg for ochratoxin A and 2 μg/kg for zearalenone.

High Pressure Liquid Chromatographic Determination of Sulfanitran and Dinsed in Medicated Feeds and Premixes

1977 ◽  
Vol 60 (5) ◽  
pp. 1064-1066
Author(s):  
Kathleen L Eaves ◽  
Billy M Colvin ◽  
Alan R Hanks ◽  
Rodney J Bushway
Keyword(s):  
High Pressure ◽  
Colorimetric Method ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Method ◽  
Medium Porosity ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple reverse phase high pressure liquid chromatographic method is described for determining sulfanitran (acetyl-p-nitrophenylsulfanilamide) and Dinsed (dinitrodiphenylsulfonylethylenediamine) in a variety of feed premixes and formulations. Feed premixes are extracted with dimethylformamide, and formulated feeds are extracted with hot methanol. The extract is filtered through medium porosity paper and injected into a liquid chromatograph equipped with a 254 nm ultraviolet detector and a 30 cm column packed with μBondapak C18. The mobile phase is acetonitrile-water (45+55) at a flow rate of 1.0 ml/min. Chromatography was complete in 10 min and peak heights were used for quantitation. Comparison of analyses of commercial samples by this method and by the AOAC colorimetric method, 42.176–42.179, showed close agreement. Recovery of spiked feed samples ranged from 98 to 105%. Butynorate and roxarsone, 2 other drugs which are normally found in combination with sulfanitran and Dinsed, do not interfere.

High Pressure Liquid Chromatographic Determination of Monensin in Feed Premixes

1983 ◽  
Vol 66 (2) ◽  
pp. 284-286
Author(s):  
Thomas D Macy ◽  
Andrew Loh
Keyword(s):  
High Pressure ◽  
Coefficient Of Variation ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Average Recovery ◽  
Bioassay Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method has been developed to determine monensin in feed premixes. The method is simple and rapid. Monensin is extracted with methanol-water and determined in the extracting solution by HPLC. Average recovery for monensin from a 13.2% premix sample was 103% (coefficient of variation (CV), 2.6%) by HPLC and compares with the value of 100% (CV, 3.4%) obtained by the turbidimetric bioassay method.

High Pressure Liquid Chromatographic Determination of Nitrofurazone in Milk

1979 ◽  
Vol 62 (1) ◽  
pp. 19-22 ◽  
Author(s):  
Arnost B Vilim ◽  
Agnes I Macintosh
Keyword(s):  
High Pressure ◽  
Screening Method ◽  
Chromatographic Determination ◽  
Organic Layer ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Milk Serum ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid high pressure liquid chromatographic (HPLC) screening method for the quantitative determination of nitrofurazone in milk has been developed. The drug is extracted with ethyl acetate from a 2.0 ml milk serum sample, the organic layer is evaporated to dryness, and the residue is dissolved in the mobile phase and injected into the liquid chromatograph. A reverse phase μBondapak C18 column is used with monitoring at 365 nm. The detection limit is 5 ppb and recoveries are 57—67%. Mass spectroscopic confirmation of the HPLC nitrofuran peak is described.

High Pressure Liquid Chromatographic Determination of Ethopabate in Feeds

1977 ◽  
Vol 60 (5) ◽  
pp. 1048-1050
Author(s):  
Leonard R Schronk ◽  
Billy M Colvin ◽  
Alan R Hanks ◽  
Rodney J Bushway
Keyword(s):  
High Pressure ◽  
Limit Of Detection ◽  
Colorimetric Method ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Hplc Method ◽  
Detector Response ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method is described for determining ethopabate in poultry feeds. Feed samples containing ethopabate are finely ground, extracted 30 min by sonification with methanol-water (80+20), and filtered. The extract is cleaned up on an alumina column, and the first 4 ml eluate collected is analyzed. The drug is eluted through a μBondapak C18 column with acetonitrile-water (30+70) at a flow rate of 1.4 ml/min and detected by ultraviolet absorption at 280 nm. Chromatography is complete in 7 min, and detector response is linear. The drug is quantitated by peak height ratios. The procedure described is reproducible and shows good agreement with the official AOAC colorimetric method. The lower limit of detection is 2 ng by HPLC, making the method applicable to residue analyses.

High Pressure Liquid Chromatographic Determination of Xanthomegnin in Corn

1978 ◽  
Vol 61 (3) ◽  
pp. 590-592
Author(s):  
Michael E Stack ◽  
Nathan L Brown ◽  
Robert M Eppley
Keyword(s):  
High Pressure ◽  
Silica Gel ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
High Pressure Liquid Chromatograph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Layer Chromatography

Abstract A method is described for the detection and quantitative analysis of xanthomegnin in corn samples. Initial extraction with CHCI3 in the presence of 0.5M H3PO4 is followed by additional purification using silica gel column chromatography. A high pressure liquid chromatograph equipped with a microparticle silica gel column and a 405 nm absorbance detector is used for detection and quantitation of the xanthomegnin. The identity of xanthomegnin is confirmed by thin layer chromatography on silica gel plates developed with benzenemethanol- acetic acid (90-(-5+5). The recovery of xanthomegnin added to corn samples at levels of 0.75–9.6 mg/kg averaged 41% with a coefficient of variation of 25%.

High Pressure Liquid Chromatographic Determination of Naphthaleneacetamide Residues in Apples

1980 ◽  
Vol 63 (1) ◽  
pp. 145-148
Author(s):  
William P Cochrane ◽  
Monique Lanouette ◽  
Ralph Grant
Keyword(s):  
High Pressure ◽  
Flow Rate ◽  
Chromatographic Determination ◽  
Accurate Method ◽  
Naphthaleneacetic Acid ◽  
High Pressure Liquid Chromatographic ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, rapid, and accurate method has been developed for the determination of naphthaleneacetamide (NAAmide) residues in apples. After extraction with chloroform, separation is performed on an RP-8 high pressure liquid chromatographic column using acetonitrile-water (30 + 70) buffered to pH 3.5 at a flow rate of 1.7 mi/min. Either a variable wavelength ultraviolet detector set at 220 nm or a fluorometric detector can be used for quantitation. Average recoveries at the 0.01 and 0.1 ppm spiking levels were 83 and 89%, respectively. Incorporation into a previously described method for naphthaleneacetic acid (NAA) residues in apples has resulted in a procedure for the simultaneous determination of NAA and NAAmide.

High Pressure Liquid Chromatographic Determination of Sucrose in Honey

1977 ◽  
Vol 60 (4) ◽  
pp. 838-841 ◽  
Author(s):  
James E Thean ◽  
Walter C Funderburk
Keyword(s):  
High Pressure ◽  
Membrane Filter ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Field Samples ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Refractive Index Detector

Abstract A normal phase high pressure liquid chromatographic (HPLC) method is presented for separating and determining sucrose in honeys. This method has been successfully applied to the analysis of field samples containing sucrose (0.63–8.44 wt %). Diluted honeys are filtered through a 0.45 μm membrane filter, and injected directly into the chromatograph. Samples are eluted from a μBondapak/carbohydrate column with acetonitrile-water (83+17) and quantitated with a refractive index detector. Average recovery of sucrose is 97%.

Reverse Phase High Pressure Liquid Chromatographic Determination of Vitamin K1 in Infant Formulas

1983 ◽  
Vol 66 (5) ◽  
pp. 1063-1066
Author(s):  
Martin P Bueno ◽  
Melina C Villalobos
Keyword(s):  
High Pressure ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
Vitamin K1 ◽  
Infant Formulas ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A reverse phase high pressure liquid chromatographic (HPLC) method for quantitating vitamin K1 in enzymatic hydrolysates of infant formula is described. The vitamin is extracted with n-pentane before determination by isocratic and isothermal reverse phase HPLC. Recovery of vitamin Ki added io 5 infant formulas ranged from 84 to 103%

High Pressure Liquid Chromatographic Determination of Uncombined Intermediates and Subsidiary Colors in Orange B

1977 ◽  
Vol 60 (5) ◽  
pp. 1067-1069
Author(s):  
Manjeet Singh
Keyword(s):  
High Pressure ◽  
Thin Layer ◽  
Sulfonic Acid ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A high pressure liquid chromatographic (HPLC) method has been developed for isolating and determining uncombined intermediates and subsidiary colors in Orange B. Samples of Orange B containing 0.1–0.3% naphthionic acid, 0.05–0.2 % phenylhydrazine-p-sulfonic acid, 0.2–0.8% pyrazolone-T and ethyl ester of pyrazolone-T, 0.2–1.0% 3-[(4-sulfo-l-naphthalenyl)-azo]-4-amino-l-naphthalenesulfonic acid, and 0.1–6.0% Orange K were prepared and analyzed by using this method. Recoveries ranged from 95 to 103%, except for the phenylhydrazine-p-sulfonic acid which ranged from 95 to 140%. Ten samples of Orange B were analyzed by conventional column and thin layer chromatographic methods as well as by the HPLC method. Good agreement was obtained for naphthionic acid, Orange K, and naphthionic acid plus the naphthionic acid subsidiary.

High Pressure Liquid Chromatographic Determination of Pentachlorophenol by Using Paired Ion Chromatography Reagents

1979 ◽  
Vol 62 (5) ◽  
pp. 1004-1006
Author(s):  
Elmer H Hayes
Keyword(s):  
High Pressure ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Steel Column ◽  
Stainless Steel Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method for determining pentachlorophenol in formulations is described. Samples containing pentachlorophenol are accurately weighed in suitable volumetric flasks and diluted with dioxane. The sample is then injected onto a stainless steel column containing μBondapak C18. The mobile phase is 60% methanol/PIC A and 40% water/PIC A. This method is simple and eliminates many of the extractions required in other methods of analysis.

Sign in / Sign up

Export Citation Format

Share Document