Simultaneous determination of Fe, P, Ca, Mg, Zn, and Cu in whole blood by two-jet plasma atomic emission spectrometry.

Availability of many biological samples in ample quantity for biomedical investigations sometimes is very restricted. Therefore, there is the need for the simple techniques allowing the analysis of small amount samples. In the present work the two-jet plasma atomic emission spectrometry techniques for the determination of Fe, P, Ca, Mg, Zn, and Cu in whole blood are proposed. The first technique is developed for direct analysis of freeze-dried blood. The sample preparation consisted in a dilution of blood powder (particle size 20 microm or less) with a spectroscopic buffer (graphite powder containing 15 wt.% NaCl). For the analysis of liquid whole blood, previous carbonization (not ashing) of blood evaporated on graphite powder was applied. Calibration samples based on graphite powder containing 15 wt.% NaCl were used. The validation of the techniques was confirmed by the use of different sample preparation procedures (wet acid digestion and dry carbonization), the analysis of IAEA A-13 reference material (freeze-dried bovine whole blood), and the comparison of the results obtained by the proposed technique with the results of the stripping voltammetry technique. Just 20-50 microL of whole blood is quite enough for all determinations. The proposed techniques were successfully applied for the simultaneous determination of Fe, P, Ca, Mg, Zn, and Cu in whole blood of living experimental rats and mice and human blood.

Determination of trace elements in bone by two-jet plasma atomic emission spectrometry.

This paper describes an analytical method for trace element determination in bone tissues. The study of the influence of the bone matrix showed that the addition of 25% ground bone to graphite powder with introduced impurities did not affect the analytical signal of elements in the spectral excitation in a two-jet plasma. On basis of these investigations a method for direct multielement analysis of bone tissues was suggested. The sample preparation procedure consisted in mixing powdered bone (particle size 30 µm or less) with a spectroscopic buffer (graphite powder plus NaCl) in ratio 1:3 or to a greater extent depending on the analyte concentration. Reference samples based on graphite powder were used for construction of calibration curves. The NaCl concentration in analyzed and calibration samples was 15 wt%. The effect of particle size was revealed from the determination of Ba, Sr, and Mg. To eliminate this effect, treatment of the samples with nitric acid was proposed. The validation of the technique was confirmed by comparison of the analysis results of a bone sample with those obtained by inductively coupled plasma atomic emission spectrometry after wet acid digestion. The limits of detection estimated for 20 elements were the following (µg g(-1)): 0.1 (Ag), 1.0 (Al), 1.0 (Ba), 0.1 (Be), 1.2 (Bi), 0.4 (Cd), 1.0 (Co), 0.2 (Cu), 0.6 (Cr), 1.9 (In), 2 (Fe), 0.3 (Ga), 0.4 (Mn), 0.4 (Mo), 0.7 (Ni), 1.0 (Pb), 0.7 (Sn), 0.8 (Tl), 5 (Sr), 1.0 (Zn).