Determination of Benzo (a) pyrene in Foods

1978 ◽  
Vol 61 (1) ◽  
pp. 129-135
Author(s):  
Yukio Saito ◽  
Hiroshi Sekita ◽  
Mitsuharu Takeda ◽  
Mitsuru Uchiyama
Keyword(s):  
Sulfuric Acid ◽  
Silica Gel ◽  
Column Chromatography ◽  
Analytical Method ◽  
Selective Extraction ◽  
Acid Extraction ◽  
Simple Method ◽  
Extraction Step ◽  
Concentrated Sulfuric Acid

Abstract An analytical method was developed for determining benzo (a) pyrene in foods, suitable for routine use. The method consists of 4 cleanup steps: (1) alkali cleavage of sample, (2) preliminary silica gel column chromatography, (3) selective extraction with concentrated sulfuric acid, and (4) further silica gel column chromatography. Recoveries of benzo- (a) pyrene added to 50 g (or 10 g) food at levels of 0.4 ppb (or 2 ppb) ranged from 70% for short-necked clam and mackerel to 85% for chicken meat. The sulfuric acid extraction step affords a simple method for isolating benzo (a)- pyrene from various kinds of interfering substances which could not be separated by existing methods.

scholarly journals Comparison of Cleanup Techniques for Simple Method for Analysis of Selected Organophosphorus Pesticide Residues in Molluscs

1996 ◽  
Vol 79 (1) ◽  
pp. 123-131 ◽  
Author(s):  
Félix Hernández ◽  
Roque Serrano ◽  
Joaquim Beltran ◽  
Francisco J López
Keyword(s):  
Silica Gel ◽  
Column Chromatography ◽  
Pesticide Residues ◽  
High Speed ◽  
Mytilus Galloprovincialis ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Gas Chromatograph ◽  
Simple Method

Abstract A simple method for determination of 5 organo phosphorus pesticides (dimethoate, chlorfenvin phos, chlorpyrifos, methidathion, and phosmet) in molluscs (Mytilus galloprovincialis and Venus gallina) was developed, with special attention to cleanup. Organophosphorus pesticides were extracted with acetonitrile-acetone (90 + 10, v/v) in a high-speed blender. Two cleanup procedures were used to defat extracts prior to injection into a gas chromatograph: liquid-liquid partition with acetoni trile-hexane and adsorption column chromatography with silica gel. The latter was more efficient for elimination of fat and fractionation of pesticides with different polarities. Limits of detection of the overall procedure including extraction and cleanup ranged from 0.2 to 1 ng/g. Quantitative recoveries for pesticide concentrations ranging from 1 to 10 000 ng/g were obtained.

A Headspace Gas Chromatographic Method for Determination of Formic acid Content in Isosulfan Blue and in Various Drugs

2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

A sensor for the in situ determination of acidity levels in concentrated sulfuric acid

1999 ◽  
Vol 365 (4) ◽  
pp. 310-313
Author(s):  
B. Hammouti ◽  
H. Oudda ◽  
A. El Maslout ◽  
A. Benayada
Keyword(s):  
Sulfuric Acid ◽  
Concentrated Sulfuric Acid

Determination of Microgram Quantities of Inorganic Boron in Mammalian Specimens

1965 ◽  
Vol 11 (3) ◽  
pp. 378-385 ◽  
Author(s):  
T Konikowski ◽  
Lee E Farr
Keyword(s):  
Cerebrospinal Fluid ◽  
Sulfuric Acid ◽  
Boron Concentration ◽  
Clinical Chemistry ◽  
Mammalian Tissue ◽  
Mammalian Tissues ◽  
Concentrated Sulfuric Acid ◽  
Reference Graph

Abstract A method is presented for estimation of inorganic boron in mammalian tissues, blood, cerebrospinal fluid, and urine. The procedure is simple and rapid, qualifying it particularly to meet needs in clinical chemistry. The mammalian tissues are first enzymatically digested and extracted; then the deproteinized extract is allowed to react with quinalizarin in concentrated sulfuric acid. The intensity of the resultant color is read spectrophotometrically at 620 mµ. The boron concentration in the tissue analyzed is obtained from a standard reference graph for that tissue. The method is applicable to concentrations as low as I µg. of boron per gram of mammalian tissue or fluid.

Liquid Chromatographic Determination of Polycyclic Aromatic Hydrocarbons in Fish and Shellfish

1985 ◽  
Vol 68 (5) ◽  
pp. 945-949
Author(s):  
Keigo Takatsuki ◽  
Shigeru Suzuki ◽  
Nobutoshi Sato ◽  
Isamu Ushizawa
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Silica Gel ◽  
Aromatic Hydrocarbons ◽  
Ethyl Ether ◽  
Analytical Method ◽  
Alkaline Digestion ◽  
Polycyclic Aromatic ◽  
Liquid Chromatographic ◽  
Fish And Shellfish

Abstract A simple and accurate analytical method for determination of polycyclic aromatic hydrocarbons (PAHs) in fish and shellfish is presented, which is considered to be useful for routine analyses and for screening purposes. The procedure involves alkaline digestion, extraction with n-hexane, silica gel column chromatography, and liquid chromatographic (LC) determination with fluorometric detection. During development of the analytical method for determination of PAHs, it was found that benzo[a]pyrene, a representative PAH, was decomposed easily by the analytical procedure, and this tendency was investigated for the experimental conditions used. Benzo[a]pyrene was decomposed by the coexistence of alkaline conditions, light, and oxygen; by peroxides in aged ethyl ether; and by oxygen when adsorbed on silica gel. Thus, to obtain good recoveries and precise analytical results, these decomposition conditions must be avoided. The following precautions are recommended: protection from light through all analytical steps; addition of Na2S to alkaline digestion mixture as an antioxidant; complete removal of peroxides from ethyl ether just before use; quick column chromatography on silica gel; and prevention of air from contact with adsorbent. When this simple method was applied to fish and shellfish samples, very good recoveries of PAHs from fortified fish samples were obtained, and no serious interferences were observed in fish and shellfish extracts

A simple method for purifying silica gel for column chromatography

1988 ◽  
Vol 65 (10) ◽  
pp. 891 ◽  
Author(s):  
Antonio E. Guarconi ◽  
Victor F. Ferreira
Keyword(s):  
Silica Gel ◽  
Column Chromatography ◽  
Simple Method

scholarly journals A Headspace Gas Chromatographic Method for Determination of Formic Acid Content in Isosulfan Blue and Various Drug Substances

2021 ◽  
Vol 37 (02) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

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