Abstract
This work describes a procedure for determination of Cd, Ni and V in spices by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) using direct solid sampling (SS). The use of Pd/Mg(NO3)2 as modifier for Cd, and an additional air-assisted pyrolysis step allowed the use of aqueous calibration for all analytes. Accuracy was checked by analysis of certified reference materials (CRMs) and the results were in agreement to certified values at 95% confidence level (t-test). Eight samples of spices were analyzed by the proposed procedure and by inductively coupled plasma mass spectrometry (ICP-MS). The found concentrations were 88-233 ng g-1 Cd , 113-2842 ng g-1 Ni and 154-1007 ng g-1 V, with precision generally better than 12%. Results obtained by the proposed procedure were in agreement with those obtained by microwave-assisted digestion and ICP-MS determination. The limits of detection were 0.2, 18 and 7 ng g-1 for Cd, Ni and V, respectively.
Highlights
The solid sampling (SS) HR-CS graphite furnace atomic absorption spectrometry (GF AAS) has been employed for elemental analysis in a wide variety of matrices including plastic materials and polymers,[13,14,15] carbon-based materials,[10,16,17,18] plant materials,[19,20] food samples,[21,22,23] and biological samples,[24,25,26] this technique is still unexplored for trace element analysis in food additives
Paprika, nutmeg, ginger, garlic, wasabi, saffron and cinnamon in dried and ground forms were purchased at a local market in São Carlos (SP, Brazil)
One of the most interesting features in SS-GF AAS is the possibility of using aqueous calibration to analyze
Summary
Spices are defined as pungent substances obtained from dried seeds, roots, barks, fruits or vegetables which are primarily used for flavoring, coloring, preserving and disguising some off-flavors in foods.[1,2] It can be added to foods in different forms such as whole spices, ground spices, essential oils and infusions.[3,4] Among several components, spices may contain both essential and toxic trace metals in a wide concentration range, originated from the raw material, contamination or adulteration sources.[4,5] In order to ensure the safety and quality control of those food additives, the development of accurate and sensitive analytical methods for determination of trace elements is essential. Direct solid sampling (SS) coupled to graphite furnace atomic absorption spectrometry (GF AAS) is attractive for determination of trace metals due to its high sensitivity, minimal use of hazardous and toxic reagents, least sample handling and reduced risks of contamination or. The performance of the proposed procedure was checked by analyzing solid certified reference materials (CRMs) and by comparison with inductively coupled plasma mass spectrometry (ICP-MS) after sample digestion in a microwave oven. An Agilent 8800 inductively coupled plasma tandem mass spectrometer (ICP-MS/MS) with a triple quadrupole (Agilent Technologies, Tokyo, Japan) was used to perform the comparative analysis. Further details about this instrument and its features can be found elsewhere.[28]. Paprika, nutmeg, ginger, garlic, wasabi, saffron and cinnamon in dried and ground forms were purchased at a local market in São Carlos (SP, Brazil)
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