Determination of Biogenic Amines in Beers and Their Raw Materials by Ion-Pair Liquid Chromatography with Postcolumn Derivatization

1993 ◽  
Vol 76 (5) ◽  
pp. 1027-1032 ◽  
Author(s):  
M L Izquierdo-Pulido ◽  
M C Vidal-Carou ◽  
A Marine-Font
Keyword(s):  
Biogenic Amines ◽  
Raw Materials ◽  
Reversed Phase ◽  
Ion Pair ◽  
Simple Preparation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Fluorescent Derivatives ◽  
Postcolumn Derivatization

Abstract A liquid chromatographic method is described for the determination in one run of the following 10 biogenic amines in beers: histamine, tyramine, serotonin, (β-phenylethylamine, tryptamine, cadaverine, putrescine, agmatine, spermine, and spermidine. The method is based on ion-pair chromatographic partition on a reversed-phase column and involves a postcolumn reaction with o-phthalaldehyde (OPT) to form fluorescent derivatives with amines. Treatment of beer samples before injection requires only a filtration through a 0.45 μm filter. It is necessary to obtain a perchloric extract for analysis of raw materials (malt and hops). The method was tested for lack of interference from amino acids and other amines. Linearity, precision, recovery, and sensitivity were satisfactory. Detection limits ranged from 0.30 to 0.40 mg/L, and determination limits ranged from 0.40 to 0.50 mg/L, except for serotonin and spermine, which were slightly higher. The simple preparation of sample and the automatic accomplishment of derivatization steps considerably reduce analysis time and effort.

scholarly journals Determination of Biogenic Amines in Cheese

1997 ◽  
Vol 80 (5) ◽  
pp. 1006-1012 ◽  
Author(s):  
Silvana R Vale ◽  
M Beatriz A Glória
Keyword(s):  
Hydrochloric Acid ◽  
Biogenic Amines ◽  
Reversed Phase ◽  
Fluorometric Detection ◽  
Acid Extraction ◽  
Ion Pair Chromatography ◽  
Liquid Chromatographic ◽  
Postcolumn Derivatization ◽  
Ml Detection

Abstract A liquid chromatographic (LC) procedure for determining 10 biogenic amines in cheese is described. The method is based on ion-pair chromatography on a reversed-phase column with postcolumn derivatization with o-phthaldialdehyde and fluorometric detection. It allowed simultaneous determination of 10 amines in <80 min: histamine, tyramine, tryptamine, 2-phenylethylamine, serotonin, agmatine,spermine, spermidine, putrescine, and cadaverine. Linearity for each amine was observed between 0.5 and 6.0 μg/mL. Detection limits ranged from 0.004 to 0.009 μg/20 μL, and determination limits ranged from 0.066 to 0.149 mg/100 g. Amino acids and other amines did not interfere with determination of biogenic amines. Three extractantsmethanol, hydrochloric acid, and trichloroacetic acidwere compared in their efficiency to recover aminesfrom spiked samples. Purification of the cheese extract was required prior to LC to avoid interference from compounds in the cheese matrix. Hydrochloric acid extraction followed by purification with diethyl ether gave best recoveries for all the amines (75.5-112.3%). The method is simple, fast, and reliable. It can be used to study the technological and toxicological implications of biogenic amines in cheeses.

scholarly journals Liquid Chromatographic Determination of S-Adenosyl-L-Methionine in Dietary Supplement Tablets

2002 ◽  
Vol 85 (4) ◽  
pp. 901-905 ◽  
Author(s):  
Joseph Ziqi Zhou ◽  
Ted Waszkuc ◽  
Spiro Garbis ◽  
Felicia Mohammed
Keyword(s):  
Dietary Supplement ◽  
Phosphate Buffer ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Ion Pair ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and reliable liquid chromatographic method was developed for the determination of S-adenosyl-L-methionine (SAM) in dietary supplement tablets. SAM in products was extracted with a phosphate buffer and separated from the mixture on a reversed-phase C8 column by ion-pair chromatography. A gradient mobile phase containing phosphate buffer, sodium octanesulfonate as the ion-pair reagent, and acetonitrile at a flow rate of 1.2 mL/min was used in the analysis. The UV detection wavelength was set at 257 nm. The calibration curve was linear over a range of 75–375 μg/mL for the SAM active ion with R2 = 0.9999. Replicate tests indicated good reproducibility of the method with a relative standard deviation of 0.9% (n = 8). The multiple extractions and recoveries from fortified products showed the high accuracy of the analysis. The use of the acidic buffer for SAM extraction and elution and the use of a fresh standard for each calibration to counteract the instability of the SAM compound significantly improved the accuracy of the method.

Liquid Chromatographic Method for Determination of Biogenic Amines in Fish and Fish Products

1995 ◽  
Vol 78 (4) ◽  
pp. 1045-1050 ◽  
Author(s):  
María Teresa Veciana-Nogues ◽  
Teresa Hernandez-Jover ◽  
Abel Marine-Font ◽  
María Del Carmen Vedal-Carou
Keyword(s):  
Biogenic Amines ◽  
Chromatographic Method ◽  
Frozen Storage ◽  
Short Term ◽  
Fish Products ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Postcolumn Derivatization

Abstract A liquid chromatographic method with postcolumn derivatization is described for determination of biogenic amines in fish and fish products. Histamine, tyramine, serotonin, β-phenylethylamine, tryptamine, putrescine, cadaverine, agmatine, spermine, and spermidine can be determined in less than 60 min. Routine sample preinjection treatment implies only 2 extractions with 0.6N perchloric acid and filtration through a 0.45 μm filter. Lack of interferences from volatile amines, amino acids, and dipeptides was verified. Results of reliability study were satisfactory. The proposed method was linear for each amine between 0.25 and 8.00 mg/L. Average recoveries ranged from 92 to 103%. Precisions (coefficients of variation) ranged from 0.70 to 9.75%. Determination limits were ≤1 mg/kg. A modification in LC conditions was necessary to apply the method to ripened fish products to avoid interferences from food matrixes. In addition, stability of biogenic amines in fresh anchovies and hake during short-term frozen storage was studied. Results showed that, except for agmatine, frozen storage is suitable for keeping samples before analysis.

Liquid Chromatographic Determination of Amiodarone Hydrochloride and Related Compounds in Raw Materials and Tablets

1994 ◽  
Vol 77 (6) ◽  
pp. 1447-1453 ◽  
Author(s):  
Pauline M Lacrok ◽  
Norman M Curran ◽  
Wing-Wah Sy ◽  
Dennis K J Goreck ◽  
Pierre Thibault ◽  
...  
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Amiodarone Hydrochloride ◽  
Related Compounds

Abstract A liquid chromatographic method for the determination of amiodarone hydrochloride and 10 related compounds in drug raw material and for assay of drug in tablets was developed. The method specifies a 3 jxm Hypersil nitrile column (150 × 4.6 mm), a mobile phase of 1 + 1 acetonitrile–ammonium acetate buffer (0.1 M adjusted to pH 6.0 with 0.1 M acetic acid), a flow rate of 1 mL/min, and detection at 240 nm. The lower limit of quantitation of the related compounds is 0.02% or less. Drug contents in 2 raw material samples were 100.1 and 99.9% and ranged from 98.2 to 99.4% in 3 tablet formulations. Impurity levels in 2 samples of raw material from different manufacturers were ca 0.4%. The presence of 3 of the known related compounds in these samples was confirmed by liquid chromatographymass spectrometry. The method applied to raw materials was evaluated by a second laboratory and found to be satisfactory.

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