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Plasma samples (n = 155) of 30 patients on an intensive ward were analysed for magnesium simultaneously by atomic absorption spectrophotometry (AAS) and methylthymol blue spectrophotometry. Methylthymol blue spectrophotometry was performed at the bedside, using two different multianalysers, Easy ST 1 and Easy ST 2, Merck, D-Darmstadt. Precision was 12.2% (Easy ST 1) and 17.1% (Easy ST 2), and the average value was 0.89 mmol/l, which was above the expected range (0.72-0.88 mmol/l). Accuracy was 16.25% (Easy ST 1) and 8.75% (Easy ST 2). Analyser 2 was more accurate (8.75% versus 6.25%) but less precise (17.1% versus 12.2%) than analyser 1. Precision of AAS was between the expected values of 0.69 and 0.84 mmol/l. Easy ST and AAS gave significantly different values (p < 0.0001) for 155 measurements. Comparison of AAS and methylthymol blue spectrophotometery showed that methylthymol blue spectrophotometry produced higher values than AAS (mean difference 0.186 mmol/l). Furthermore, analyses of 40 samples of a standardized plasma concentration with methylthymol blue spectrophotometry showed a very low precision (15.3%). Easy ST cannot be assigned for urinary measurements of magnesium. Experimentally measured samples gave unaccountable results.
A simple and rapid method is described for the determination of lead in foods. The samples are digested in HNO3, HF, and HClO4 and then the lead is determined by atomic absorption spectrophotometry using an electrothermal atomizer with the L'vov platform. Interferences and ways to improve the precision and accuracy of the analysis were studied. Matrix modification using 1% ammonium phosphate alleviated most interferences encountered. The precision and accuracy of the method was evaluated using NBS SRM 1570 Spinach and SRM 1566 Oyster Tissue. The values obtained are in good agreement with the certified values.
Graphite furnace atomic absorption spectrophotometry was used to determine chromium and molybdenum in 7 medical foods from 5 manufacturers. Linear standard curves were obtained for both elements for concentrations between 5 and 25 ng/mL. Detection limits were 0.24 ng/mL for Cr and 0.67 ng/mL for Mo. Characteristic masses were 3.1 and 14.7 pg for Cr and Mo, respectively. No difference was detected between wet and dry ashing methods, and dry ashing was used to complete the study. The method was validated by assaying various National Institute of Standards and Technology standard reference materials. Analysis of these products for Cr and Mo were within certified values. One product was evaluated by this method for reproducibility (n = 5). Relative standard deviations were 6.8 and 4.8% for Cr and Mo, respectively. This product contained 0.31 +/= 0.02 micrograms Cr/g and 0.63 +/- 0.03 micrograms Mo/g. The remaining products contained 0.09-1.28 micrograms Cr/g and 0.07-2.3 micrograms Mo/g. Mean recovery values were 98 +/- 14% (n = 14) for Cr at spike levels of 0.20-1.89 micrograms/g and 102 +/- 24% (n = 10) for Mo at spike levels of 0.30-1.89 micrograms/g.
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A graphite furnace atomic absorption spectrophotometry method was used to determine the total aluminum content of various foods found in an average American diet. The food products were ashed in platinum dishes, and the inorganic residue was fused using a sodium carbonate-sodium borate mixture. The fusion step allowed detection of all the various forms of aluminum found in food products. A L'vov platform was used in the graphite furnace to increase the sensitivity of the assay. Care was taken throughout the analysis to avoid various sources of aluminum contamination such as glass and porcelain dishes. All reagents were ultra-pure grade and were continuously monitored for aluminum content. Sodium borate used in the fusion flux mixture had previously been extracted with 8-hydroxyquinoline in chloroform to remove any aluminum present. Both raw and cooked foods were analyzed for aluminum with this method. Average recoveries of aluminum from food products ranged from 84 to 112%. The overall coefficient of variation of this method on the food products tested was 10%.
We describe a method of analysis for copper, cadmium, and zinc in a 15-mg (wet weight) sample of human liver by atomic absorption spectrophotometry. The sample is digested with nitric acid (1.0 mol/liter), evaporated, and dilute HNO3 (10 mmol/liter) added. The reconstituted acid mixture is injected into the graphite tube atomizer for analysis of Cu and Cd and aspirated into the air--acetylene flame for measurement of Zn. The absorbance for each metal is suppressed with increasing pH. NaNO3, KNO3, KCl, and NaCl (e.g.) quench the Cd absorbance in acid solutions that contain no protein, but not in the presence of protein. Metal ions added to the predigestion human liver sample at 10 percent and 100 percent of the intrinsic metal concentrations were, respectively, 93 percent and 90 percent accounted for analytically in the case of Cu, 98 percent and 102 percent for Zn, and 101 percent and 93 percent for Cd. Analysis of a National Bureau of Standards' Bovine Liver Standard Reference Material yielded results corresponding to 99 percent (Cu), 112 percent (Zn), and 91 percent (Cd) of the mean expected concentrations of these metals. The between-run coefficient of variation for the bovine liver material was 6 percent for Cu, 9 percent for Zn, and 10 percent for Cd. For 16 histologically normal samples of human liver, the mean values were: Cu, 26; Zn, 293; and Cd, 6.0 nanograms of metal per milligram dry weight, in agreement with values published previously. The method can be easily and reliably applied to small samples of liver obtained by closed-needle biopsy.
A flameless atomic absorption method for the coextraction of platinum and palladium from biological and environmental samples by high molecular weight amine (HMWA) is given. Also, methods for lead determination in biological samples by use of extraction flameless analysis and direct aspiration-flame analysis are reported. A study of lead contamination of Vacutainer tubes is given.
A flameless atomic absorption method was developed for the determination of mercurial preservatives in biologicals. The assay was based on a quantitative determination of the mercury content of these preservatives. This method was used to analyze a variety of samples and yielded reproducible results with satisfactory recoveries. The procedure is presented in a simplified block diagram and described in detail relating its suitability for routine assay of large numbers of samples.
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Recent development of flameless atomic absorption spectrophotometry has made possible more precise and sensitive determinations of metals including lead. This means that a sample size of microliter order of blood has come to give a sufficient analytic signal. Blood lead which has usually been determined using venous blood was determined in the present study using a small amount of capillary blood. The method developed is of lead determination in the capillary blood sample from earlobe by means of flameless atomic absorption spectrophotometry equipped with an automated microsampling system or autosampler. Thus, 70 microliters of heparinized whole blood sample from earlobe gave a satisfactory result in the lead analysis. The procedure is as follows. 1) Blood obtained from the earlobe is collected in a heparinized capillary tube. 2) The blood is diluted in the ratio of 1 : 9 with Triton 5000 X solution for complete hemolysis of erythrocytes, by which the matrix-bound lead is released and a better distribution of samples is made possible in the graphite tube. 3) Finally the sample is analyzed by a flameless atomic absorption spectrophotometer with an autosampler. Making sure the analytical method to be accurate and reliable for blood lead determination, the authors compared capillary blood lead levels (Pb-Bc) with venous ones (Pb-Bv) from the same subjects in the same sampling session. It was found that the correlation between Pb-Bc and Pb-Bv was highly significant (n = 144, r = +0.998, y = 0.97 x+0.32, p less than 0.001) and that they were almost of the same level. It was concluded that the method developed may be recommended for the routine clinical use.
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Procedures for the determination of aluminum, chromium, cobalt, nickel, and iron in whole blood are presented and discussed. Chromium, cobalt, nickel, and iron were determined from one sample after decomposition of the blood with a mixture of nitric and perchloric acids. A graphite furnace was used for the determination of chromium, cobalt and nickel, and flame AAS was used for iron. The determination of Al was done from separate samples by GFAAS after dilution with 1% Triton TX-100. The normal concentration of these elements was measured in rabbit and dog blood.
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