Journal of Pharmaceutical and Biomedical Analysis 47 (2008) 541–546
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Journal of Pharmaceutical and Biomedical Analysis
journal homepage: www.elsevier.com/locate/jpba
Use of slurry suspension sample introduction technique in fast multielement
analysis of multimineral and multivitamin formulations by inductively
coupled plasma atomic emission spectrometry
George A. Zachariadis
∗
, Agathi F. Olympiou
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki, Greece
article info
Article history:
Received 30 November 2007
Received in revised form 25 January 2008
Accepted 12 February 2008
Available online 17 February 2008
Keywords:
Metals
Slurry suspensions
Inductively coupled plasma emission
spectrometry
Multiminerals
Analysis of variance
abstract
A slurry suspension sampling technique has been developed and optimized for rapid multielemental
analysis of multivitamin/multimineral preparations using inductively coupled plasma atomic emission
spectrometry (ICP-AES). The following macro-, micro- and trace-elements: Ca, Mg, Mn, Fe, Cr, Al, Ag, B, Ba,
Bi, Cd, Co, Cu, Ga, In, Ni, Pb, Zn, As and Se were determined by the proposed method. The lower detection
limits were obtained for Mn, Mg, Cu and Ca whereas the highest for Bi, Pb, As and Se. Consequently the
method can be used as a fast screening method. A wet-acid mineralization method was applied as total
recovery method for comparative purposes. Samples were prepared as slurries at a concentration of 5%
(m/v) in aqueous acidic media (0.8 M HNO
3
). Various factors affecting the sensitivity of the method were
optimized. The obtained results were subjected to two-way analysis of variance to examine any significant
difference between the developed slurry procedure and the wet-acid complete decomposition. Finally,
the slurry suspension technique was found to be applicable in routine quality control and contamination
monitoring of multimineral preparations. For the analyzed commercial preparations, the found elemental
concentrations are compared to those appearing in the label of the products.
© 2008 Elsevier B.V. All rights reserved.
1. Introduction
Multivitamin and multimineral supplements are designed
specifically to provide a variety of essential nutrients for the body.
Multivitamin supplements can help to prevent both vitamin and
mineral deficiencies, and are used by many to increase essen-
tial nutrients in the body and achieve additional health benefits.
Multivitamins usually contain at least 100%, if not more, of the rec-
ommended dietary allowance of essential vitamins and minerals
[1]. Nutrients that are commonly included in a multivitamin prepa-
ration are: vitamins A, B-complex, C, D, E, K, and among minerals,
magnesium, zinc, calcium, iodine, selenium, copper, manganese,
chromium and molybdenum, etc. Reference daily intakes for 11
significant metallic elements have been established to the follow-
ing amounts: Ca (1000 mg), Cr (120 g), Cu (2 mg), Fe (18 mg), K
(3500 mg), Mg (400 mg), Mn (2 mg), Mo (75 g), Na (2400 mg), Se
(70 g) and Zn (15 mg) [2]. The various commercial products dif-
fer at the levels of each element and furthermore some of them
do not contain several of the necessary metals. Generally, two to
four tablets may provide the daily amount of minor nutrients like
iron and copper, but for major nutrients like calcium the amount is
∗
Corresponding author. Tel.: +30 2310997707; fax: +30 2310997719.
E-mail address: zacharia@chem.auth.gr (G.A. Zachariadis).
much lower. However these products do not replace the common
food sources but are used only as supplements.
Considering the toxicity of some elements such as chromium,
lead, cadmium, etc., inspection of their content in multivitamin
preparation is a necessity [3]. However, taking into account the
very low content of these analytes in studied preparations, analyt-
ical methods of high sensitivity should be used. On the other hand,
a suitable sample preparation procedure is usually the key step in
the whole method. Conventional wet-acid digestions [3–5] require
about 2–3 h but are typically faster than dry ashing procedures.
An alternative but less reported technique is the slurry suspen-
sion nebulization, including direct aspiration of suspended sample
into a suitable atomizer [6]. In this case, it is necessary to optimize
the aspiration and atomization conditions to obtain reproducible
results.
Various element-specific detectors have been used for the
analysis of multivitamin preparations including flame atomic spec-
trometry or graphite furnace spectrometry [7–9]. Using flame
atomic absorption spectrometry, Soriano et al. reported the acid
extraction of four nutritional elements in HCl [9] with comparable
results to the total digestion procedure. Despite of the fact that these
techniques provide good sensitivity, they are in principle single-
element detectors, thus they are not convenient for multielement
analysis of samples like multiminerals. For this reason recently,
inductively coupled plasma-based techniques coupled either with
0731-7085/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.jpba.2008.02.010