Abstract
Multivitamin/mineral (MVM) supplements possess highly saline matrix which, unless eliminated, precludes accurate determination of trace amounts of toxic metal impurities by inductively coupled plasma mass spectrometry (ICP-MS). Multi-step separations (up to four-steps) are described in literature; often for single element determinations due to difficulties in removing the matrix components. In this study, we developed a three-step sequential coprecipitation procedure for simultaneous separation of As and Cd impurities from MVM supplements for determination by ICP-MS. The procedure provided effective elimination of salt matrix, including Ca, Mg and KCl along with the interfering molybdenum (Mo) and tin (Sn) from MVM solutions. KCl, Mo and Sn were removed by two-step Mg(OH)2 coprecipitation to about 34 µg mL-1 K (ca. 31 µg mL-1 Cl) and 0.4 µg mL-1 Mo. Levels of Sn and Na were not significant. A third coprecipitation of the resulting MVM solution with HF + NH4OH mixture precipitated virtually all Ca and Mg to as low as 1 and 10 µg mL-1, respectively. The recoveries for As and Cd in the spiked MVM solutions were about 96% and 95%, respectively. The accuracy of the method was validated with analysis of multivitamin/multielement tablets certified reference material (SRM 3280). Experimental values were 112 ± 37 ng g-1 for 75As, and 76 ± 5, 79 ± 5, and 78 ± 7 ng g-1 for 110Cd, 111Cd and 114Cd isotopes, respectively, that were not significantly different from the certified values of As (132 ± 44 ng g-1) and Cd (80.2 ± 0.9 ng g-1) at 95% confidence level. Several commercially available MVM supplements were analyzed with the procedure. Mean As levels measured in the tablets varied between 24 and 128 ng g-1 and that for Cd were between 28 and 125 ng g-1 indicating total amount of As or Cd ingested per serving size were below the safe daily exposure limits. In addition, the results obtained for As and Cd with the procedure were lower in comparison to the values reported in literature indicating that ICP-MS analysis of complex MVM supplements could be prone to higher risks of inaccuracy without removal of interfering matrix.