Study for the determination of Cd, Pb and Zn - PowerPoint

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					                                           Study for the determination of Cd, Pb and Zn in biological fluids
                                                 by Inductively Coupled Plasma Mass Spectrometry

                                                       Monica Ursu1, Maria Paul1, Marin Şenilă1, Tiberiu Frenţiu2, Mircea Chintoanu1, Claudiu Tănăselia1
                                                                                                      1Institutul     de Cercetări pentru Instrumentaţie Analitică, Cluj-Napoca
                                                      2Facultatea de      Chimie şi Inginerie Chimică, Universitatea Babeş-Bolyai, Cluj-Napoca, Institutul de Cercetări pentru Instrumentaţie Analitică, Cluj-Napoca




           OJECTIVES                            INSTRUMENTATION                                                                                    RESULTS                                                                                 CONCLUSIONS
                                            The instrument used for determination
•Developing high sensitivity                 was a ICP-MS Perkin-Elmer Elan                                   The signal and also the concentration in                                                                              The method developed for urine
                                             DRC II with methane as a reaction                                     stadard mode is higher than in
analysis method for Cd, Cu, Pb                                                                                                                                                                                                       analysis based on 1+9 dilution with
                                             gas for DRC determination.                                            standard mode because of the
and Zn determination from clinical                                                                                 interference. When still using                                                                                    HNO3 1% and blood 1+19 diluted
samples (urine and whole blood)                                                                                    internal standards, this difference in                                                                            with Triton-X 0.5% is suitable for
                                                                                                                   signal strength can be seen.                                                                                      direct determination oh heavy
                                                                                                              For background evaluation determination                                                                                metals in clinical samples using
•Study of polyatomic interferences                                                                                 we used Millipore deionized water                                                                                 ICP-MS method.
removal using dynamic reaction                                                                                     with 1% nitric acid. Also, the                                                                                   Polyatomical interferences on Pb
cell method (with methane as a                                                                                     parameters of the Elan DRC II were
                                                                                                                                                                                                                                     and Zn cand be elemininating by
                                                                                                                   is the specification: the vacuum
reaction gas)                                                                                                                                                                                                                        using Dynamica Reaction Chamber
                                                                                                                   value and the signal intesities for
                                                                                                                   etalons.                                                                                                          with methane as reaction gas.
                                                                                                                                                                                                                                    DRC with methane gas isnot
•Determination of analytical                                                                                                                     CRM Urine 05404 level 2
                                                                                                                                                                                                                                     suitable for interference removal of
performance of the method used,                                                                               Elem               Isoto            ppb                           measurred                          CRM conc.
                                                                                                                                                                                                                                     Cu compounds because of the
                                                                                                              ent                pe               concentration                                                    (ppb)
by analysis of certified reference                                                                                                                                                                                                   carbon ions that results in the
                                                                                                                                                  without                    with DRC
materials
                                                                   CRMs                                                                           DRC
                                                                                                                                                                                                                                     chamber. This should be further
                                                                                                              Cd                 110Cd            11.77          ±           10.33 ± 0.40                          8.00 ± 1.86
                                            For the method developing, we’ve used certified
                                                                                                                                                  0.30
                                                                                                                                                                                                                                     investigated using amonia instead of
                                              reference
                                              materials for biological fluids, from the next                                     111Cd            11.39          ±           9.30 ± 0.10
                                                                                                                                                                                                                                     methane as a reaction gas.
                                              suppliers:                                                                                          0.20
                                                                                                                                                                                                                                    The method we developed stands
                                                                                                                                 112Cd            9.62           ±           8.83 ± 0.10
                                             Urine CRM (SERO AS Norway):                                                                         0.30                                                                               for high sensitivity and allows
                                             SERONOM 201205 level 2 lot no. 02525                                               113Cd            11.34          ±           8.75 ± 0.30                                             determination of concentration in
                                             SERONOM 201305 blank lot OK4636                                                                     0.10
                                                                                                                                                                                                                                     the range of ppt (parts per trillion)
                                             LGC Prochem Germany                                                                114Cd            9.21           ±           8.85 ± 0.20
                                             Control level 2-05404                                                                               0.10
                                                                                                                                                                                                                                     from chemical samples with low
                                             Control level 1-05403 (Medichem)                                Cu                 63Cu             256 ± 24                   303 ± 18                              250 ± 60
                                                                                                                                                                                                                                     salts content (Cd – 20 ppt, Cu – 60
                                             Blood CRM:
                                                                                                                                 65Cu             256 ± 29                   286 ± 17
                                                                                                                                                                                                                                     ppt, Pb – 90 ppt, Zn – 60 ppt)
                                             SERONOM 201605 Trace Elements Whole Blood
                                              L2 Lot. No. 0503109                                             Pb                 206Pb            124 ± 35                   103 ± 25                              80 ± 18
                                                                                                                                 207Pb            121 ± 20                   105 ± 27
                                            Used reagents:
                                                                                                                                 208Pb            122 ± 18                   106 ± 22
                                             Deionized water Milli-Q, Millipore
                                             Ultrapure nitric acid 60%, Merck                                Zn                 64Zn             856 ± 59                   805 ± 47                              800 ± 200
                                             Monoelement standard solutions 1000ppm                                             66Zn             840 ± 70                   805 ± 52
                                              containing Cd, Cu, Pb, Zn (Merck)
                                             Triton X-100 1% v/v (Merck – K Ga A)
                                                                                                                                 68Zn             836 ± 34                   812 ± 34

                                             Methane (99.9995%) for reaction gas

                                              Urine sample was diluted 1+9 in 100ul HNO3
                                              60%. Following concentration were added: Cd 0.5                 CRM
                                                                                                              Urine
                                                                                                                          Cd                        Cu                          Pb                                 Zn


                                              (1) Cu 5 (10) Pb 5 (10) Zn 50 (100). For blood, we                          M             CRM         M            CRM            M                 CRM              M     CRM


                                              used 1+19 dilution with Triton X-100 1% and the                 SERON
                                                                                                              ORM
                                                                                                                          5.05
                                                                                                                          ±
                                                                                                                                        5.06 ±
                                                                                                                                        0.22
                                                                                                                                                    18.6 ±
                                                                                                                                                    0.3
                                                                                                                                                                 16.1
                                                                                                                                                                 1.4
                                                                                                                                                                        ±       85.9
                                                                                                                                                                                ± 4.2
                                                                                                                                                                                                  91.1±
                                                                                                                                                                                                  7.0
                                                                                                                                                                                                                   259
                                                                                                                                                                                                                   ±
                                                                                                                                                                                                                         261
                                                                                                                                                                                                                         13
                                                                                                                                                                                                                               ±


                                              same concentrations.                                            201205      0.10                                                                                     17


                                                                                                              05403       13.02         13.00       49.5 ±       50.0   ±       98±1              130 ±            144   1300 ±
                                                                                                                          ±             ± 3.00      5.6          14.8           0                 32               5 ±   400
                                                                                                                          0.25                                                                                     74


                                                                                                              05404       9.21          8.00 ±      256 ±        250    ±       103               80      ±        807   800   ±

                                                       ANALITICAL                                                         ±
                                                                                                                          0.30
                                                                                                                                        1.86        29           60             ± 25              18               ±
                                                                                                                                                                                                                   40
                                                                                                                                                                                                                         200



                                                                                                              OK4636                                19.0 ±       18.6   ±                                          384   393   ±



 Fig 1. Quadrupole chamber (foreground)               PERFORMANCE                                                                                   1.4          2.1                                               ±
                                                                                                                                                                                                                   25
                                                                                                                                                                                                                         28




        and DRC (background)                                          LOD/ppt    RPq



                                                           Cd110      9          0.3                                                             Urine CRM sample
                                                           Cd111      6          0.45
                                                                                                                                                                                                                                     Fig. 3: DRC opened (detail).
                                                           Cd112      5          0.35


                                                           Cd113      4          0.25


                                                           Cd114      4          0.35


                                                           Cu63       12         0.45
                                                                                                                       Whole Blood CRM 201605 level 2 lot no. 0503109
                                                           Cu65       20         0.6

                                                           Pb206      29         0.35
                                                                                                               Cd                         Cu                            Pb                                    Zn                   Pentru informaţii suplimentare:
                                                                                                               M          CRM             M              CRM            M               CRM                   M          CRM

                                                           Pb207      25         0.55
                                                                                                               5.8 ±
                                                                                                               0.1
                                                                                                                          6.0 ±
                                                                                                                          0.4
                                                                                                                                          684±
                                                                                                                                          36
                                                                                                                                                         666 ±
                                                                                                                                                         29
                                                                                                                                                                        402 ±
                                                                                                                                                                        33
                                                                                                                                                                                        393
                                                                                                                                                                                        21
                                                                                                                                                                                              ±               5304 ±
                                                                                                                                                                                                              174
                                                                                                                                                                                                                         5038 ±
                                                                                                                                                                                                                         369
                                                                                                                                                                                                                                   INCDO-INOE 2000
                                                           Pb208      16         0.60
                                                                                                                                                                                                                                   Institutul de Cercetări pentru
                                                           Zn64       12         0.45
                                                                                                                         Whole blood determination results                                                                         Instrumentaţie Analitică, ICIA
                                                           Zn66       20         0.45                                                                                                                                              Str. Donath 67, Cluj-Napoca 400293.
                                                           Zn68       17         0.45                                                                                                                                              E-mail: icia@icia.ro


 Fig. 2. Perkin-Elmer Elan DRC II with
         qudrupole region in foreground.