Elimination of Spectral Interferences for the Determination of Fe and Se in Biological Samples Using ICP-Ion Trap Mass Spectrometer

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1 BUNSEKI KAGAKU Vol. 54, No. 5, pp. 373 _ The Japan Society for Analytical Chemistry 1 R 1 Elimination of Spectral Interferences for the Determination of Fe and Se in Biological Samples Using ICP-Ion Trap Mass Spectrometer Jun HORIGOME 1 and Naoki FURUTA 1 1 Department of Applied Chemistry, Faculty of Science and Engineering, Chuo University, , Kasuga, Bunkyo-ku, Tokyo (Received 25 November 2004, Accepted 1 March 2005) An inductively coupled plasma mass spectrometer with an ion-trap mass spectrometer was used for the determination of Fe and Se in biological samples. The spectral interferences of Ar 2, P 2 O, 12 C 35 Cl 2 and 32 S 16 O 3 on 78 Se, 80 Se and 82 Se were eliminated by optimizing the ion level and FNF (filtered noise field) function of 3DQMS (three dimensional quadrupole mass spectrometer). As a result of decreasing Ar 2, a linearity of 7 orders of magnitude from 100 ppt to 100 ppm and a limit of detection of 11 ppt were achieved at 80 Se. The spectral interferences of Ar 16 O, Ca 16 O, 79 Br 1 H and 81 Br 1 H decreased by using the CID (collision induced dissociation) function of 3DQMS. The optimum conditions of CID obtained from the signal intensity and the isotopic ratio of Fe and Se were 0 V and 500 ms. Under the optimum conditions of the ion level, FNF and CID, Se in human urine standard materials (NIES CRM 18 and Seronorm 2524) was determined ; the analytical results showed good agreement with reference values within the analytical error, and a recovery of 101 could be attained for Fe in human urine standard material (Seronorm 2524). The developed method enabled us to determine Se and Fe in biological samples by using the most abundant isotopes of 56 Fe and 80 Se. Keywords : inductively coupled plasma ; ion-trap mass spectrometer ; spectral interferences ; biological samples ; ICP-3DQMS. 1 ICP-MS QMS ICP 1 : ICP-MS 3DQMS 1) QMS 2) 3DQMS P-5000 ICP-3DQMS 3)6)

2 374 BUNSEKI KAGAKU Vol QMS 0.1 2) 3DQMS 1) QMS 7)9) 10)11) ICP CaO H 2 12) Fe ICP-QMS 56 Fe Ar 16 O Ca Ca 16 O Se 6 Ar ICP-QMS Se 12)18) ICP-3DQMS Se Fe Fe Se 3DQMS ms s 2 21 P-5000 Hitachi High- Technologies Co. 3DQMS 3 3DQMS m/z filtered noise fieldfnf m/z 3DQMS ICP-MS Ar Ar 3DQMS collision induced dissociationcid m/z 3DQMS He FNF CID 3DQMS 22 Fe Se Table 1 m/z DQMS Ar Ar 3DQMS Ar Table 1 FNF 3DQMS

3 : ICP- MS Fe Se 375 Table 1 Operating conditions for ICP-3DQMS instruments Instrumental parameters RF power 10 W plasma Ar flow 14 l min l auxiliary Ar flow 1.2 l min l nebulizer Ar flow 1.3 l min l up-take rate 0.4 ml min l buffer gas He buffer gas pressure 2.5 kg f/cm 2 internal standard 59 Co, 115 In measurement times 5 times Ion trap parameters 56 Fe 80 Se ion level 42 amu 56 amu filtered noise field amu amu FNF voltage 4.4 V 5.0 V Table 2 Spectral interferences on the determination of Fe and Se in biological samples by ICP-MS Isotope Abundance, Interferences 54 Fe Fe Fe Fe Se Se Se Se Se Se 8.73 Ar 14 N, 38 Ar 16 O, Ca 14 N Ar 16 O, Ca 16 O Ar 16 O 1 H, Ca 16 O 1 H Ar 16 O 1 H 1 H, Ca 16 O 1 H 1 H 37 Cl 2, Ar 34 S 36 Ar Ar, 38 Ar 38 Ar, Ar 36 S, 31 P 14 2 N Ar 37 Cl, Ar 36 Ar 1 H 38 Ar Ar, 31 P 16 2 O Ar Ar, 32 S 16 O 3, 1 H 79 Br 12 C 35 Cl 2, 34 S 16 O 3, Ar 1 2 H 2, 1 H 81 Br Table 1 FNF Se 1000 ppmspex Fe 1000 ppm 0.1 M HNO 370 Fe Se Table 2 56 Fe Ar 16 O Ca 16 O 78 Se 80 Se 82 Se Ar 2 31 P 16 2 O 79 Br 1 H 81 Br 1 H 32 S 16 O 3 12 C 35 Cl 2 CaBrPS Cl ppm Table 3 Matrix solutions prepared for this study Element Conc./ppm Interferences Ca (CaCO 3) 100 Ca 16 O S (H 2SO 4) S 16 O 3, 34 S 16 O 3 Br (KBr) 10 1 H 79 Br, 1 H 81 Br C, Cl (HCl, CH 3COOH) 00, C 35 Cl 2 P (H 3PO 4) P 16 2 O Table M HNO 3 Ar 16 O Ar NIES CRM 18 human urine (National Institute for Environmental Studies, Tsukuba, Japan), Seronorm trace elements human urine 2524 (Sero As, Bllingstad, Norway), NIST bovine liver SRM 1577 a (National Institute of Standards and Technology, Gaithersburg, MD, USA) 233 Milestone MLS 1200 Milestone, Sorisole, Italy PTFE NIST SRM g 3 ml HNO 3 1mlH 2O W5 min20 W1 min3250 W5 min4 0 W 5 min5600 W5 min 50 ml 0.1 M HNO 3 10 g NIES CRM 18 Seronorm Se 311 Ar 2 QMS HP-4500Agilent Technologies, Tokyo, Japan Fig. 1a QMS Ar cps 3DQMS Fig. 1b3DQMS Ar 2 10 cps Ar 2 80 Se

4 376 BUNSEKI KAGAKU Vol Fig. 1 Comparison of blank (0.1 M HNO 3) spectra obtained by ICP-QMS and ICP-3DQMS (a): ICP-QMS (HP4500); (b): ICP-3DQMS Fig. 2 Matrix effect on the background signal intensity (without Se ; trapping time : 500 ms ; accumulation times : 100 times) : m/z 78 ; : m/z 80 ; : m/z ppt100 ppm ppt10 ppb100 ms ; 100 ppb1 ppm10 ms ; 10 ppm1 ms; 100 ppm0.1 ms 11 ppt Ar 2 FNF FNF Ar Ar 2 Ar Fig. 2 Se m/z Se Br 79 Br 1 H 81 Br 1 H BrH m/z 80 2 ppbm/z ppb P 2O SO 3 CCl 2 3 He Br BrH

5 : ICP- MS Fe Se 377 Table 4 Determination of Se in biological certified reference materials without CID Found/ng g 1 with CID Reference/ng g 1 CRM CRM CRM CRM 1 : Seronorm trace elements human urine 2524 (10-fold dilution); CRM 2 : NIES CRM 18 human urine (10-fold dilution); CRM 3 : NIST SRM 1577 bovine liver (-fold dilution); CID : 0 V, 500 ms ; Trapping time : 500 ms ; Accumulation times : 30 times Fig. 3 Selenium isotope ratio as a function of CID time (CID : 0 V ; Se : 10 ng g 1 ; trapping time : 500 ms ; accumulation times : 50 times) (a): 80/78 ; (b): 82/78 ; : without Br ; : 10 µg g 1 Br CID BrH 80 Se 82 Se BrH 3DQMS CID Fig. 3 CID BrH CID 0V CID 0msBr BrH Br m/z Br 1 H 81 Br 1 H CID BrH BrH CID CID 500 ms BrH Se CID 0V500 ms Se 314 CID Se Table 4 CID Se Se 5 CRM1 : NIES CRM 18 CRM 2 : Seronorm 2524 CRM3 : NIST SRM 1577CRM12 Se 3DQMS CID CRM3 Se Br CID 32 Fe 321 3DQMS Fe Ar 16 O Ca 16 O Ca Ca 100 ppm 3DQMS Fig. 4 Ar 16 O 15 ppb Ca 16 O 45 ppb Ca 100 ppm m/z 57 Ca 16 OH Ar 16 O Ca Ca 16 O 3DQMS CID 322 CID ArO CaO Fig. 5 CID Ar 16 O Ca 16 O CID Fe 100 ppb Fe 100 ppb Ca 100 ppm Ca 100 ppm CID 0msCa Ca 16 O Ca CID Ca 16 O CID 500 ms Ca 16 O Fe Fig. 6 Fe 100 ppbca 100 ppm Fe

6 378 BUNSEKI KAGAKU Vol Fig. 4 Mass spectra obtained by ICP-3DQMS (trapping time : 50 ms ; accumulation times : 100 times) (a): blank (0.1 M HNO 3); (b): 100 µg g 1 Ca ; :blank (0.1 M HNO 3); : 100 µg g 1 Ca 323 CID Fe Fe Fe Table 5 Seronorm 2524 Fe Fe CID Ar 16 O Ca 16 O 100 Fig. 5 Signal intensity of Fe as a function of CID time (CID : 0 V ; trapping time : 50 ms ; accumulation times : 100 times) ----: blank (0.1 M HNO 3); ----: 100 µg g 1 Ca ; : 100 ng g 1 Fe ; : 100 ng g 1 Fe100 µg g 1 Ca 100 ppbca 100 ppm CID CID 0V500 ms CID Ca 16 O Ca 16 O 20 Ca 16 OH Ca 16 O CID 0V500 ms Fe Fe 73.6 ppb Fe ppb 4 3DQMS FNF 78 Se 80 Se 82 Se 31 P 16 2 O Ar 2 32 S 16 O 3 12 C 35 Cl 2 56 Fe Ar 16 O Ca 16 O 80 Se 82 Se 79 Br 1 H 81 Br 1 H 3DQMS CID Ar 16 O Ca 16 O 79 Br 1 H 81 Br 1 H Fe Se

7 : ICP- MS Fe Se 379 Fig. 6 Mass spectra obtained by ICP-3DQMS (trapping time : 50 ms ; accumulation times : 100 times) (a): without CID ; (b): with CID 0 V, 500 ms ; -----: blank (0.1 M HNO 3); -----: 100 µg g 1 Ca ; : 100 ng g 1 Fe ; : 100 ng g 1 Fe100 µg g 1 Ca Table 5 Determination of Fe in Seronorm trace elements human urine 2524 and recovery test CID 0V500 ms FNF CID NIES CRM 18 Seronorm 2524 Se Seronorm 2524 Fe 101 Fe Se Fe Se 56 Fe 80 Se without CID with CID Fe concentrattion Before addition/ng g Added/ng g After addition/ng g Recovery, CID : 0 V, 500 ms ; Trapping time : 100 ms ; Accumulation times : 30 times 1) N. Furuta, A. Takeda, J. Zheng, T. Nabeshima : Evaluation of Inductively Coupled Plasma - Ion Trap Mass Spectrometry, in Plasma Source Mass Spectrometry, Edited by G. Holland, S. D. Tanner, p. 90 (2001), (Royal Society of Chemistry). 2),,, : (Bunseki Kagaku), 6, 527 (2004). 3) G. C. Eiden, C. J. Barinaga, D. W. Koppenaal : J. Anal. At. Spectrom., 11, 317 (1996). 4) D. W. Koppenaal, C. J. Barinaga, M. R. Smith : J. Anal. At. Spectrom., 9, 1053 (1994). 5) G. C. Eiden, C. J. Barinaga, D. W. Koppenaal : J. Am. Soc. Mass Spectrom., 7, 1161 (1996). 6) C. J. Barinaga, D. W. Koppenaal : Rapid Comm. Mass Spctrm., 8, 71 (1994). 7) N. S. Nonose, N. Matsuda, N. Fudagawa, M. Kubota : Spectrochimica Acta, 49B, 955 (1994). 8) K. Sakata, K. Kawabata : Spectrochimica Acta, 49B, 1027 (1994). 9) S. D. Tanner : J. Anal. At. Soectrom., 10, 905 (1995). 10) D. W. Koppenaal, G. C. Eiden, C. J. Barinaga : J. Anal. At. Spectrom., 19, 561 (2004). 11) S. D. Tanner, V. I. Baranov, D. R. Bandura : Spectrochimica Acta, 57B, 1361 (2002). 12) L. H. Reyes, J. M. M. Gayon, J. I. G. Alonso, A. Sanz- Medel : J. Anal. At. Spectrom., 18, 11 (2003). 13) B. Gammelgaard, O, Jons and L. Bendahl : J. Anal. At. Spectrom., 16, 339 (2001). 14) J. M. Marchante-Gayon, I. Feldmann, C. Thomas, N. Jakubouski : J. Anal. At. Spectrom., 16, 457 (2000). 15) B. Gammelgaard, O. Jons : J. Anal. At. Spectrom., 14, 867 (1999). 16) L. C. Clark, G. F. Combs, B. W. Turnbull, E. H. Slate, D. K. Charlker, J. Chow, L. S. Davis, R. A. Glover, G. F. Graham, E. G. Gross, A. Krograd, J. L. Lesher, H. K. Park, B. B. Sanders, C. L. Smith, J. R. Talor : J. Am. Med. Assoc., 276, 1957 (1996). 17) R. F. Burk, K. E. Hill, J. A. Awad, J. D. Morrow, T. Kato, K. A. Cockell, P. R. Lyons : Hepatology, 21, 561 (1995). 18) M. S. Alaejos, C. D. Romero : Clin. Chem., 39, 20 (1993).

8 380 BUNSEKI KAGAKU Vol Fe Se Fe Se 3DQMS filtered noise fieldfnf 78 Se 80 Se 82 Se Ar 2 31 P 16 2 O 32 S 16 O 3 12 C 35 Cl 2 Ar 2 80 Se 100 ppt100 ppm 7 11 ppt 3DQMS collision induced dissociationcid Ar 16 O Ca 16 O 79 Br 1 H 81 Br 1 H Fe Se CID 0V500 ms FNF CID NIES CRM 18 Seronorm 2524 Se Seronorm 2524 Fe 101 Fe Se 56 Fe 80 Se

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