Trace Analysis of Zearalenone and/or Zearalanol in Animal Chow by High Pressure Liquid Chromatography and Gas-Liquid Chromatography

1977 ◽  
Vol 60 (2) ◽  
pp. 272-278 ◽  
Author(s):  
Claude L Holder ◽  
Charles R Nony ◽  
Malcolm C Bowman
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
Silica Gel ◽  
High Pressure Liquid Chromatography ◽  
Additional Data ◽  
Gas Liquid Chromatography ◽  
Step Procedure ◽  
Rf Values ◽  
Solvent Systems ◽  
Layer Chromatography

Abstract An analytical method is described for determining residues of the estrogens zearalenone and/or zearalanol in animal chow at levels as low as 10 ppb. The chow is extracted with methanol and cleaned up by a 3-step procedure employing a Sephadex LH-20 column, liquid-liquid partitioning at pH 13 and 8.3, and a silica gel column. Residues of the 2 compounds, separated on silica gel, are assayed by using high pressure liquid chromatography with ultraviolet detection. Additional data are also included concerning p-values of the compounds in several solvent systems, Rf values from thin layer chromatography with 9 solvent systems, solubilities in 3 solvents, and a procedure for preparing their pentafluoropropionyl derivatives for analysis by electron capture gas-liquid chromatography.

Determination of Zearalenone in Cornflakes and Other Corn-Based Foods by Thin Layer Chromatography, High Pressure Liquid Chromatography, and Gas-Liquid Chromatography/High Resolution Mass Spectrometry

1978 ◽  
Vol 61 (3) ◽  
pp. 593-600
Author(s):  
Peter M Scott ◽  
Thavil Panalaks ◽  
Sri Kanhere ◽  
Walter F Miles
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Pressure Liquid Chromatography ◽  
Limit Of Detection ◽  
Gas Liquid Chromatography ◽  
Natural Occurrence ◽  
Layer Chromatography

Abstract A simple cleanup procedure based on pH adjustments was used to obtain extracts of corn foods. The method gave good recoveries of zearalenone determined by thin layer chromatography (TLC) and high pressure liquid chromatography (HPLC). As little as 5 ng zearalenone was detected by TLC, using Fast Violet B Salt as the spray reagent; the lower limit of detection in cornflakes was about 20 ≧kg. With HPLC on Spherisorb silica (5 ≧m) and detection by fluorescence at an excitation maximum of 310 nm as little as 5 ≧g zearalenone/kg cornflakes could be determined. While the TLC method was also applicable to corn chips, cornmeal, popcorn, and frozen corn, an interference was observed in HPLC of the latter 3 products. This interference was separated from zearalenone by adding a second HPLC analytical column (Spherisorb ODS). Gas-liquid chromatography coupled with mass spectrometric single ion monitoring at high resolution, although of limited availability, was shown to be the most sensitive and selective method for determining zearalenone in corn foods. The natural occurrence of zearalenone in a sample of cornflakes (13–20 ≧/kg) was demonstrated by all 3 detection procedures.

scholarly journals Ekstraksi, Karakterisasi dan Uji Aktivitas Antioksidan Astaxanthin dari Produk Fermentasi Udang (Cincalok)

2021 ◽  
Vol 24 (3) ◽  
pp. 311-322
Author(s):  
Mauludia Mauludia ◽  
Thamrin Usman ◽  
Winda Rahmalia ◽  
Dwi Imam Prayitno ◽  
Siti Nani Nurbaeti
Keyword(s):  
Antioxidant Activity ◽  
High Pressure ◽  
Liquid Chromatography ◽  
High Pressure Liquid Chromatography ◽  
Aquatic Organisms ◽  
Dpph Method ◽  
Wet Weight ◽  
Tlc Analysis ◽  
Layer Chromatography

Shrimp is one of the aquatic organisms that contain several active compounds, including astaxanthin. Cincalok is one of the fermented shrimp products containing astaxanthin. This study aims to determine the characteristics of astaxanthin extract from cincalok and its antioxidant activity. Extraction of astaxanthin from cincalok was carried out using the reflux method with acetone : cyclohexane (20:80 v/v) as a solvent. The identification and characterization of astaxanthin was carried out using thin-layer chromatography (TLC), UV-Vis spectrophotometry, and High-Pressure Liquid Chromatography (HPLC). Meanwhile, the antioxidant activity test was carried out using the 1,1-diphenyl-2-picrylhydrazyl (DPPH) method in one serial concentration (5; 15; 25 ppm). The results of TLC analysis showed that astaxanthin in cincalok extract has Rf value (0.32). The analysis using a UV-Vis spectrophotometer produced a spectrum with a maximum wavelength of 477 nm, which corresponds to the maximum wavelength of standard astaxanthin. The yield of astaxanthin extract from cincalok in this study was 1.47 mg/100 g wet weight. The chromatogram from the results of UHPLC analysis showed that the retention time of cincalok astaxanthin extract was 6.27 minutes with a purity of 18.03%. The antioxidant activity of cincalok astaxanthin extract was 568.32 ppm. Udang merupakan salah satu organisme air yang mengandung banyak senyawa aktif, termasuk astaxanthin. Cincalok merupakan salah satu produk hasil fermentasi udang yang mengandung astaxanthin. Penelitian ini bertujuan untuk mengetahui karakteristik ekstrak astaxanthin dari cincalok dan aktivitas antioksidannya. Ekstraksi astaxanthin dari cincalok menggunakan metode refluks dengan pelarut aseton:sikloheksan (20:80 v/v). Identifikasi dan karakterisasi astaxanthin dilakukan dengan menggunakan kromatografi lapis tipis (KLT), spektrofotometri UV-Vis, dan High Pressure Liquid Chromatography (HPLC). Sedangkan uji aktivitas antioksidan dilakukan menggunakan metode 1,1-difenil-2-pikrilhidrazil (DPPH) dengan memvariasikan konsentrasi larutan uji, yaitu 5; 15; 25 ppm. Hasil dari penelitian ini melaporkan astaxanthin pada ekstrak cincalok menunjukkan nilai Rf 0,32 pada kromatografi lapis tipis (KLT). Hasil analisis menggunakan spektrofotometer UV-Vis menghasilkan spektra dengan panjang gelombang maksimum 477 nm, yang sesuai dengan panjang gelombang maksimum astaxanthin standar. Randemen ekstrak astaxanthin dari cincalok pada penelitian ini adalah 1,47 mg/100 g berat basah. Kromatogram dari hasil analisis UHPLC menunjukkan waktu retensi ekstrak astaxanthin cincalok yaitu selama 6,27 menit dengan kemurnian sebesar 18,03%. Aktivitas antioksidan dari ekstrak astaxanthin cincalok diperoleh sebesar 568,32 ppm.  

Additional Cleanup of Samples on GLC Column for TLC Determination of Pesticide Residues

1967 ◽  
Vol 50 (3) ◽  
pp. 615-623
Author(s):  
Kenneth T Hartman
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pesticide Residues ◽  
Gas Liquid Chromatography ◽  
Rf Values ◽  
Layer Chromatography

Abstract Gas-liquid chromatography (GLC) following conventional isolation procedures has been used to clean up pesticide residues for confirmation by thin layer chromatography (TLC). This procedure is more rapid and efficient than present cleanup procedures and permits the determination of pesticide residues that do not survive these rigorous acid or alkali treatments. The method also permits TLC confirmation of pesticide residues that have similar Rf values but different GLC retention times. Recoveries ranged from 85 to 105% for 25 of 28 pesticides tested

Quantitation of the Contaminants in Technical Fenitrothion by Reverse Phase High Pressure Liquid Chromatography

1979 ◽  
Vol 62 (6) ◽  
pp. 1222-1230
Author(s):  
William P Cochrane ◽  
Monique Lanouette ◽  
Roy Greenhalgh
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
High Pressure Liquid Chromatography ◽  
The Other ◽  
Average Level ◽  
Uv Detector ◽  
Reverse Phase ◽  
Technical Grade ◽  
Solvent Systems

Abstract Technical grade samples of fenitrothion were analyzed by high pressure liquid chromatography (HPLC) on a reverse phase LiChrosorb RP-8 column, using 3 solvent systems and a UV detector set at 269 nm. All commercial samples analyzed contained >94% fenitrothion; in addition, 9 contaminants were identified and quantitated. Bisfenitrothion was the major contaminant, with average amounts of 2.46% from one manufacturer and 1.17% from another. The second most abundant toxicant was S-methyl fenitrothion, which was present at an average level of 0.71% in one source but only 0.16% in the other. The amount of fenitrooxon was 0.046% or less in samples from 2 manufacturers. Other contaminants quantitated include the 2 demethyl fenitrothion isomers, 3-methyl-4-nitrophenol, 3-methyl-6-nitrophenol, 3-methyI-4-nitroanisole, and bis-S-methyl fenitrothion. The total amount of the constituents quantitated in 9 commercial samples was 99.07 ± 1.81%. By comparing the amounts of bis-fenitrothion and phenols present in technical grade fenitrothion, it should be possible to identify the specific manufacturers of the various products.

High-Pressure Liquid Chromatography of Benzo (a) pyrene and Benzo(ghi)perylene in Oil-Contaminated Shellfish

1976 ◽  
Vol 59 (5) ◽  
pp. 989-992 ◽  
Author(s):  
Humberto Guerrero ◽  
Edward R Biehl ◽  
Charles T Kenner
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Silica Gel ◽  
High Pressure Liquid Chromatography ◽  
High Pressure Liquid Chromatographic ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic ◽  
Polynuclear Aromatics

Abstract A high-pressure liquid chromatographic procedure is described for the determination of benzo (a) pyrene and benzo(ghi)perylene. These polynuclear aromatics are extracted with acetonitrile and partitioned into petroleum ether, the petroleum ether is removed, and the residue is saponified. The compounds are purified and isolated by passing the residue through a silica gel column and a high-pressure liquid chromatographic column, and detected by their ultraviolet absorption. Recoveries of standards through the procedure averaged 104%.

An improved synthesis of m-diazirinophenol

1984 ◽  
Vol 62 (9) ◽  
pp. 1767-1771 ◽  
Author(s):  
Pierre Leblanc ◽  
Gerhard E. Gerber
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
Silica Gel ◽  
High Pressure Liquid Chromatography ◽  
Good Yield ◽  
Reverse Phase ◽  
Oxidation Step ◽  
Work Up

The published synthesis of phenolic diazirine was shown to result in products which were chlorinated during the hypochlorite oxidation while the desired unchlorinated product was lost during the usual work-up. A superior synthesis is described: inclusion of pyridine during the oxidation step prevents the chlorination; the desired volatile diazirine was isolated in good yield using silica gel and reverse phase high pressure liquid chromatography.

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