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 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 Aldicarb, Aldicarb Sulfoxide, and Aldicarb Sulfone in Potatoes

1981 ◽  
Vol 64 (3) ◽  
pp. 724-728
Author(s):  
William P Cochrane ◽  
Monique Lanouette
Keyword(s):  
High Pressure ◽  
Methylene Chloride ◽  
Chromatographic Determination ◽  
Enzymatic Oxidation ◽  
High Pressure Liquid Chromatographic ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract An ion-suppression reverse phase high pressure liquid chromatographic method is described for the determination of aldicarb, aldicarb sulfoxide, and aldicarb sulf one in potatoes. Samples are extracted with methylene chloride and Na2SO4, evaporated to dryness, and cleaned up using Sep-Pak silica and Sep-Pak-C18 cartridges. The extract can be successfully analyzed by high pressure liquid chromatography on either a μLiChrosorb RP-18 or μBondapak C18 column and quantitated using a variable wavelength ultraviolet detector set at either 220 or 247 nm. The mobile phase is acetonitrile-buffer (4 + 96) and (30 + 70), buffered to pH 7.6 and flowing at 2 mL/min. Recoveries ranged from 80 to 100%. The minimum detectable amount was 37.5 ng, which easily permitted the quantitation of 0.1 ppm aldicarb sulfone in 75 g sample. The recovery of aldicarb was low because of its rapid enzymatic oxidation to aldicarb sulfoxide and sulfone.

High Pressure Liquid Chromatographic Determination of Cholesterol in Foods

1981 ◽  
Vol 64 (1) ◽  
pp. 54-57 ◽  
Author(s):  
David R Newkirk ◽  
Alan J Sheppard
Keyword(s):  
High Pressure ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Chromatographic Techniques ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic method that uses the benzoate ester of cholesterol has been developed for the measurement of cholesterol in foods. A 300 × 3.9 mm id μBondapak C18 column and a variable wavelength ultraviolet detector are used with a 100% methanol mobile phase. Amounts as low as 10 ng cholesterol benzoate can be detected. The results from the analyses of a variety of foods are given and compared with results from gas-liquid chromatographic analyses. The comparison of the 2 chromatographic techniques is favorable.

Ion Pairing High Pressure Liquid Chromatographic Determination of Amaranth in Licorice Products

1981 ◽  
Vol 64 (6) ◽  
pp. 1411-1413
Author(s):  
William J Hurst ◽  
James M Mckim ◽  
Robert A Martin
Keyword(s):  
High Pressure ◽  
Ion Pairing ◽  
Chromatographic Determination ◽  
Buffer Solution ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic method is described for the determination of amaranth (FD&C Red No. 2; Red No. 2) in licorice products. The Red No. 2 is extracted with a basic buffer solution, cleaned up on a Sep-Pak column, chromatographed on a reverse phase column in the ion pairing mode, and detected at 254 nm. The procedure is time-conservative with accurate and precise results. Recovery data ranged from 93 to 104%, and coefficients of variation were less than 4% for standards and samples.

High Pressure Liquid Chromatographic Determination of Oxazepam Dosage Forms: Collaborative Study

1983 ◽  
Vol 66 (4) ◽  
pp. 864-866
Author(s):  
Eileen S Bargo ◽  
◽  
E Aranda ◽  
C Bonnin ◽  
S Hauser ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A reverse phase high pressure liquid chromatographic method for the determination of oxazepam in tablets and capsules was collaboratively studied by 9 laboratories. Collaborators were supplied with 6 samples that included synthetic and commercial formulations. Tablet and capsule composites are diluted with methanol and filtered. Oxazepam is determined at 254 nm by using a C18 column. Mean recoveries of oxazepam from synthetic tablet and capsule formulations were 97.2 and 99.0%, respectively. Mean coefficients of variation for tablets and capsules ranged from 1.85 to 2.86%. The method has been adopted official first action.

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 Uncombined Intermediates and Subsidiary Colors in FD&C Blue No. 2

1975 ◽  
Vol 58 (1) ◽  
pp. 48-49 ◽  
Author(s):  
Manjeet Singh
Keyword(s):  
High Pressure ◽  
Sulfonic Acid ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high-pressure liquid chromatographic method is presented for the isolation and determination of uncombined intermediates and subsidiary colors in FD&C Blue No. 2 (indigotine, C.I. No. 73015). Samples of FD&C Blue No. 2 containing 0.1–0.3% isatin, 0.1–0.3% isatin 5-sulfonic acid, 0.1–5.0% monosulfonated indigo, and 1.0–18.0% 5,7’-disulfonated indigo were prepared and analyzed by using this method. Recoveries ranged between 92 and 102%.

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.

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