scholarly journals A Method for Determination of Selenium in Organic Tissues Using Microwave Digestion and Liquid Chromatography

2007 ◽  
Vol 90 (3) ◽  
pp. 838-843 ◽  
Author(s):  
Espen Govasmark ◽  
Mark G Grimmett
Keyword(s):  
Certified Reference Materials ◽  
Microwave Digestion ◽  
Digestion Method ◽  
Laboratory Procedure ◽  
Liquid Chromatograph ◽  
Wet Digestion ◽  
Fluorescence Determination ◽  
Liquid Chromatographic ◽  
Selenium Analysis

Abstract An existing laboratory procedure for selenium analysis using open-vessel wet digestion and liquid chromatographic fluorescence determination was modified for use with microwave digestion. The proposed microwave digestion method eliminated the hazards associated with the use of HCIO4 while maintaining excellent recoveries of selenium. A 2-step HNO3/H2O2 digestion procedure was developed. Digested samples were derivatized with 2,3-diaminonaphthalene, and the resultant piazselenol complex was measured fluorometrically using a liquid chromatograph. Measured values were in agreement with 9 different certified reference materials. The detection limit for this method was 0.54 ng Se/g tissue (3 ), and the calibration curve remained linear (r2 = 0.9968) up to 2 g Se/g.

scholarly journals Determination of Lead, Cadmium, Zinc, Copper, and Iron in Foods by Atomic Absorption Spectrometry after Microwave Digestion: NMKL1 Collaborative Study

2000 ◽  
Vol 83 (5) ◽  
pp. 1189-1203 ◽  
Author(s):  
Lars Jorhem ◽  
Joakim Engman ◽  
B-M Arvidsson ◽  
B Åsman ◽  
C Åstrand ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Tissue Sample ◽  
Certified Reference Materials ◽  
Microwave Digestion ◽  
Collaborative Study ◽  
Absorption Spectrometry ◽  
Relative Standard ◽  
Cadmium Zinc

Abstract A method for determination of lead, cadmium, zinc, copper, and iron by atomic absorption spectrometry (AAS) after microwave digestion was subjected to a collaborative study in which 16 laboratories participated [including users of inductively coupled plasma (ICP) and ICP–mass spectrometry (MS)]. The types of samples included in the study were minced fish, wheat bran, milk powder, bovine and pig liver, mushroom, 2 simulated diets, and bovine muscle; the last 4 were certified reference materials. These were analyzed as single (4 samples), double blind (1 sample), or split level (2 samples) samples. Before the collaborative study, a pretrial was conducted in which 4 ready-made solutions and one fish tissue sample were analyzed for Pb and Cu. The reproducibility relative standard deviation (RSDR) values, for results above the detection limit, ranged from 59% at 0.155 mg/kg to 16% at 1.62 mg/kg for Pb, from 28% at 0.0124 mg/kg to 11% at 0.482 mg/kg for Cd, from 9.3% at 35.3 mg/kg to 1.7% at 147 mg/kg for Zn, from 39% at 0.241 mg/kg to 3.0% at 63.4 mg/kg for Cu, and from 17% at 7.4 mg/kg to 5.9% at 303 mg/kg for Fe. The RSDR values agreed well with the norms described by the International Union of Pure and Applied Chemistry. As a complement to the AAS determinations, a number of laboratories analyzed the samples either by ICP or by ICP–MS. The results of these analyses agreed well with the AAS results. On the basis of the results of the collaborative study, the method was adopted Official First Action by AOAC INTERNATIONAL.

Wet Oxidation Method for the Determination of Submicrogram Quantities of Mercury in Cereal Grains

1972 ◽  
Vol 55 (5) ◽  
pp. 951-959 ◽  
Author(s):  
M Malaiyandi ◽  
J P Barrette
Keyword(s):  
Vanadium Pentoxide ◽  
Cereal Grains ◽  
Acid Mixture ◽  
Wet Oxidation ◽  
Digestion Method ◽  
Oxidation Method ◽  
Digestion Procedure ◽  
Wet Digestion ◽  
Cereal Flour

Abstract A simple and rapid wet-digestion procedure is described in which flour samples containing bound and unbound mercury are decomposed, using a sulfuric-nitric acid mixture in the presence of small amounts of vanadium pentoxide. Fortification studies with 3 organomercuric compounds on mixed cereal flour indicate average recoveries in excess of 96% in the 20–500 ppb range. This wet digestion method is compared with the Klein procedure to illustrate the advantages and significance of the vanadium pentoxide oxidation.

Adaptation of a Dry Ashing Procedure for Determination of Selenium by Fluorimetry in High-Fat Foods

1995 ◽  
Vol 78 (2) ◽  
pp. 477-479 ◽  
Author(s):  
Jacques R Bellanger
Keyword(s):  
Magnesium Nitrate ◽  
High Fat ◽  
Fluorimetric Determination ◽  
Digestion Method ◽  
Wet Digestion ◽  
Dry Ashing ◽  
Selenium Determination ◽  
Wet Ashing ◽  
Total Procedure

Abstract The wet ashing–dry ashing procedure for destruction of organic matter in high-fat foods for subsequent fluorimetric determination of selenium was investigated. Samples were decomposed by predigestion with nitric acid and dry-ashed with magnesium nitrate and hydrochloric acid. Selenium was recovered quantitatively through the total procedure. Detection limit was about 4 ppb. Accuracy was tested by analysis of several reference materials and by comparison with the wet-digestion method. The present method can be used conveniently for selenium determination in high-fat foods.

Determination of thiamin and thiamin phosphate esters in blood by liquid chromatography with post-column derivatization.

1983 ◽  
Vol 29 (12) ◽  
pp. 2073-2075 ◽  
Author(s):  
M Kimura ◽  
Y Itokawa
Keyword(s):  
High Performance ◽  
Sodium Hydroxide Solution ◽  
Potassium Ferricyanide ◽  
Phosphate Esters ◽  
High Performance Liquid Chromatograph ◽  
Liquid Chromatograph ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Thiamin Pyrophosphate

Abstract We demonstrate a liquid-chromatographic method involving post-column derivatization for determining the concentration of thiamin and its phosphate esters in human blood. Blood, erythrocytes, or plasma is deproteinized and centrifuged. Aliquots of the samples are applied to a mu Bondapak C18 column attached to a "high-performance" liquid chromatograph. Addition of potassium ferricyanide/sodium hydroxide solution to the column effluent with a proportioning pump converts thiamin phosphates into fluorophores, the intensities of which are measured with a spectrofluorophotometer. Thiamin, thiamin monophosphate, thiamin pyrophosphate, and thiamin triphosphate eluted as single peaks; no coeluting substances were detected. Thiamin pyrophosphate was the ester present in greatest concentration, followed by thiamin triphosphate; thiamin monophosphate and thiamin were present in slight amounts. This method allows easy determination of thiamin and its phosphate esters in 0.1 mL of blood.

Determination of Ten Trace Element in River Deposit by ICP-OES

2013 ◽  
Vol 807-809 ◽  
pp. 196-199
Author(s):  
Ting Ting Liu ◽  
Hong Yuan Shen
Keyword(s):  
Trace Element ◽  
Standard Addition ◽  
Measured Data ◽  
Good Precision ◽  
Icp Oes ◽  
Digestion Method ◽  
Wet Digestion ◽  
Relative Standard ◽  
Precision And Accuracy

Wet digestion method had been used in river deposit of BZ profile. At the same time, Mn, Cu, Ba, Ni, Pb, Zn, Rb, V, Sr and Zr in river deposit were determined by ICP-OES. The results show that the relative standard deviations are all below 0.39%, while the recovery of standard addition is 94.3%~117.1%. The method is proved to have good precision and accuracy, and to be simple and rapid. And the measured data provide basis for paleoflood study in this area.

Liquid Chromatographic Determination of Bendiocarb in Technical Materials and Wettable Powder Formulations: Collaborative Study

1986 ◽  
Vol 69 (5) ◽  
pp. 908-911
Author(s):  
Peter L Carter ◽  
Keith C Overton ◽  
◽  
P G Baker ◽  
O O Bennett ◽  
...  
Keyword(s):  
Statistical Data ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Liquid Chromatograph ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for determination of bendiocarb in technical materials and wettable powders was tested by 12 collaborators. Bendiocarb is dissolved in acetonitrile containing 0.1% propiophenone as internal standard. This solution is analyzed on a liquid chromatograph utilizing a reverse phase (C18) column. The compound is detected at 254 nm and peak area is used for quantitation. The 3 different materials studied contained 20, 80, and nominally 100% bendiocarb. Each was examined in duplicate to provide the necessary matched pairs. Collaborators approved of the ease and simplicity of the method and, in particular, the way the method can be applied to automatic injection assemblies. The statistical data show acceptable precision of the method: Reproducibility coefficients of variation were 20% material, 2.04%; 80% material, 1.02%; and nominal 100% material (technical product), 0.64%. The method has been adopted official first action.

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