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File: Dietary Supplements Market Pdf 138145 | App Determinationofmetalsindietarysupplements
application note icp mass spectrometry authors lee davidowski ph d zoe grosser ph d laura thompson perkinelmer inc 710 bridgeport avenue shelton ct usa the determination introduction dietary supplements are ...

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                                                                                                 APPLICATION NOTE
                                                                                                 ICP-Mass Spectrometry
                                                                                                 Authors
                                                                                                  Lee Davidowski, Ph.D.
                                                                                                 Zoe Grosser, Ph.D.
                                                                                                 Laura Thompson
                                                                                                 PerkinElmer, Inc. 
                                                                                                 710 Bridgeport Avenue 
                                                                                                 Shelton, CT USA
     The Determination                                   Introduction
                                                         Dietary supplements are regulated by the FDA under the general umbrella of foods, 
     of Metals in Dietary                                but with different regulations than conventional foods. Dietary supplements have been 
     Supplements                                         defined by Congress as materials taken by mouth that include ingredients intended to 
                                                         provide dietary supplementation. They can be found in various forms, including tablets, 
                                                         powders, and liquids. They may consist of vitamins, minerals, herbs or other botanicals, 
                                                         amino acids, and substances such as enzymes, organ tissues, glandulars, and metabolites. 
                                                         Under the Dietary Supplement Health and Education Act of 1994 (DSHEA), the dietary 
                                                         supplement manufacturer is responsible for ensuring that a dietary supplement is safe 
                                                         before it is marketed. FDA is responsible for taking action against any unsafe dietary 
                                                                                                          1
                                                         supplement product after it reaches the market.  
                 One facet of ensuring a safe product is analysis of the final product before distribution. Although organic components often 
                 form the majority of a supplement, metals may be found due to their inclusion in vitamin structures such as vitamin B-12 
                 (cobalt) and minerals, such as selenium. They may also be added as a contaminant through natural products or in the manu- 
                 facturing process. The measurement of toxic metals or metals intended to be present for quality and labeling confirmation 
                 may be required. Analysis challenges include measurement at low concentrations in a variety of matrices. In this note we  
                 will use inductively coupled plasma mass spectrometry (ICP-MS) to measure a variety of elements generally considered to  
                 be hazardous to human health at low to medium concentrations. The four elements generally considered to be hazardous 
                 and not necessary for nutrition are Pb, Cd, As, and Hg. The elements Se and Cr are often added at low concentrations for 
                 nutritional purposes and were also included. 
               Experimental                                                       Arsenic analysis employed cell technology to remove the 
               Samples of a variety of commercially available protein supple-     chloride interference, arising from natural chlorine content, 
               ments representing different types of matrices were selected       salt added to a supplement material or hydrochloric acid used 
               and prepared in duplicate. Microwave digestion was used            in sample preparation, which can degrade the detection limit.  
                           ™                                                      This cell allows a gas to react with the sample and under con-
               (Multiwave  3000, PerkinElmer, Inc. Shelton, CT USA)               trolled conditions the interference is chemically separated 
               to obtain clear solutions. Six mL of nitric and 1 mL of hydro-     from the analyte. Figure 1 shows how the dynamic reaction 
                                            ™
               chloric acid (GFS Chemical , Columbus, OH  USA) were               cell (DRC) operates in removing arsenic from the chloride 
               added to PTFE vessels with approximately 0.3 g of sample and       interference by shifting the mass observed from 75 to 91.  
               the digestion program shown in Table 1 applied.  The samples       Detection limits are improved compared to other approaches 
               were then transferred and diluted to 50 mL with ASTM Type          and the precision in varying matrices is more consistent.  An 
               I water. The samples were fairly homogeneous and in a form         instrument detection limit for arsenic measured in 1000 mg/L 
               that allowed a representative sample to be easily taken. If the    NaCl was shown to be 2.3 ng/L, comparing favorably to 
               samples were chunky solids, grinding, blending or other pro-       detection limits of 0.6-1.8 ng/L, measured in 1% nitric acid 
               cedures might be necessary to ensure a more homogeneous                                            3
               sample to be measured. Preparing replicate samples will allow      solution, using this technique.
               us to evaluate if our homogeneity assumption is accurate.  
                 Table 1.  Microwave Digestion Program.
                 Step    Power (W)      Ramp (min)      Hold (min)      Fan
                 1 750  10:00  10:00  1
                 2 1200  10:00  10:00  1
                 3 0    15:00  3
                          ®                                                                                       ™
               The ELAN  DRC-e ICP-MS (PerkinElmer, Shelton, CT USA)              Figure 1.  Dynamic reaction cell (DRC ) operates with the PerkinElmer 
               was used for measurement. The instrumental conditions are          ELAN ICP-MS to react and remove interferences or to move measurement  
               shown in Table 2.                                                  to masses where interferences are not present.
                                                                                  The mass for selenium measurement was chosen to avoid 
                Table 2.  ICP-MS Instrumental Conditions.                         interference from calcium, common in dietary supplements.
                Nebulizer                        Quartz Concentric                Results and Discussion
                Spray Chamber                    Quartz Cyclonic                  Methodology developed on the ICP-MS was tested through 
                                                                                                     ®                           ®
                                                                                  analysis of a NIST  reference material NIST  1548a, Typical 
                RF Power                         1500 W                           Diet.  The sample was measured and carried through the same 
                                                                                  digestion procedure along with the supplement materials.  
                Integration time                 1000 ms (per analyte)            Table 3 shows the results obtained for Typical Diet material.
                Replicates 3                                                      The results from duplicate sample preparations are in good 
                                                                                  agreement with each other. Generally less than 20% relative 
                Reaction Gas for arsenic         O = 0.6 mL/min                   percent difference is acceptable and these range from 2-13%.  
                                                  2
                                                                                  The agreement with the certified value is within 10%, showing 
                                    91
                RPq for arsenic as  AsO 0.5                                       excellent agreement. 
       2
            Table 3.  Analysis Results, Typical Diet Reference Material (1548a).
                                 1548a – 1 (mg/kg)       1548a – 2 (mg/kg)      Average (mg/kg)  Certified Value (mg/kg)  % Rec 
            AsO 91               0.183                   0.192                  0.188                  0.20 ±0.1                    93.8
            Cd 111               0.036                   0.038                  0.037                  0.035 ±0.0015                106
            Cr 52 0.135 0.118 0.127 -                                                                                                
            Pb 208+207+206  0.045                        0.046                  0.046                  0.044 ±0.009                 104
            Hg 202               < DL                    < DL                                                                        
            Se 82                0.231                   0.251                  0.241                  0.245 ±0.028                 98.4
          Detection limits were estimated from the standard deviation of       The results for the samples are shown in Table 5. The multi-
          the blank solutions prepared using the same digestion procedure      vitamin samples contain lead, arsenic and small amounts 
          and are shown in Table 4.                                            of cadmium. These metals were not added intentionally as 
                                                                               nutritional components and may arise from contaminants in 
            Table 4.  Estimated Detection Limits.                              other whole food ingredients added to the supplement. Dolan, 
                                                                               et. al., surveyed a variety of dietary supplement products and 
                                                                                                                                   2
                                    mg/kg in supplement                        found many contain small amounts of Pb and Cd.  As long as 
                                                                               the daily dosage was not large the total amount of these metals 
            AsO 91                  0.17                                       ingested did not exceed the safe daily exposure limit.
            Cd  111                 0.0008                                     The protein powder and liquid supplement contained less of 
                                                                               the toxic elements, although the liquid supplement listed many 
            Cr 52                   0.05                                       whole food components that might be a source of contaminants.
            Pb 208                  0.01                                       A post-digestion spike on the liquid supplement (1 ppb As, 
                                                                               Cd, Cr, Pb, and Se; 0.1 ppb Hg) showed good recoveries,  
            Hg 202                  0.004                                      further supporting that both method and instrument were 
                                                                               operating as expected. 
            Se 82                   0.10
            Table 5.  Sample Results (mg/kg).
                                                                          As Cd Cr Pb Hg Se 
            Multivitamin Supplement 1                                     0.287       0.032     11.8       0.530     < DL        5.30
            Multivitamin Supplement 2                                     0.280       0.027     9.97       0.432     < DL        5.01
            Protein Powder 1                                              < DL        0.036     1.21       < DL      < DL        0.700
            Protein Powder 2                                              < DL        0.036     0.223      < DL      < DL        0.181
            Liquid Supplement                                             < DL        < DL      0.691      < DL      < DL        0.854
            Liquid Supplement Spike (% Rec)                               89.6 80.0 104 89.1 79.0  83.1
                                                                                                                                                       3
              Table 6 shows the agreement between the label claims of the 
              liquid supplement and the results obtained here for chromium 
              and selenium. The agreement between the values was good, 
              differing by only a few percent. 
                 Table 6.  Comparison with Label Claims.
                 Label Value                      Found Value This Work
                 0.676 mg/kg Cr                   0.691 mg/kg
                 0.845 mg/kg Se                   0.854 mg/kg
              Conclusion
              Measurement of trace toxic metals can help ensure dietary 
              supplement product safety. ICP-MS can be used to examine a 
              variety of metals at low concentrations. In this note, analysis 
              was used for four toxic metals and two nutritional elements 
              that can be toxic at higher concentrations. The suite of elements 
              can be easily expanded to include different elements as regula-
              tory needs evolve or metal contamination is suspected. This 
              methodology can be applied to final products or to evaluate 
              possible contamination in starting materials.
              References
              1. U.S. FDA Website 
                  http://www.cfsan.fda.gov/~dms/supplmnt.html 
              2.  Dolan, Scott P., Nortrup, David A., Bolger, P. Michael, and 
                  Capar, Stephen G., Analysis of Dietary Supplements for 
                  Arsenic, Cadmium, Mercury, and Lead Using Inductively 
                  Coupled Plasma Mass Spectrometry, J. Agric. Food Chem. 
                  2003, 51, 1307-1312.
              3. Ruth E. Wolf and Kenneth R Neubauer, Determination 
                  of Arsenic in Chloride Matrices, PerkinElmer Application 
                  Note D6357A, 2002.
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...Application note icp mass spectrometry authors lee davidowski ph d zoe grosser laura thompson perkinelmer inc bridgeport avenue shelton ct usa the determination introduction dietary supplements are regulated by fda under general umbrella of foods metals in but with different regulations than conventional have been defined congress as materials taken mouth that include ingredients intended to provide supplementation they can be found various forms including tablets powders and liquids may consist vitamins minerals herbs or other botanicals amino acids substances such enzymes organ tissues glandulars metabolites supplement health education act dshea manufacturer is responsible for ensuring a safe before it marketed taking action against any unsafe product after reaches market one facet analysis final distribution although organic components often form majority due their inclusion vitamin structures b cobalt selenium also added contaminant through natural products manu facturing process m...

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