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Supplement material to Ref. JASMS Ms. No. 2012-5464

Supplement material to Ref. JASMS Ms. No. 2012-5464 Detection of an amine impurity and quality assessment related to this impurity of the UV MALDI matrix  -cyano-4-hydroxy-cinnamic acid for the analysis of peptides in the attomole range

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Supplement material to Ref. JASMS Ms. No. 2012-5464

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  1. Supplement material to Ref. JASMS Ms. No. 2012-5464 Detection of an amine impurity and quality assessment related to this impurity of the UV MALDI matrix -cyano-4-hydroxy-cinnamic acid for the analysis of peptides in the attomole range Justyna Rechthaler, Ernst Pittenauer, Tanner M. Schaub and Günter Allmaier

  2. Legends to Figures in the Supplement Figure 1S Positive-ion MALDI mass spectra (curved field reflectron mode) of two CHCA matrix batches: matrix B (a) and matrix E (b). Matrix solvent: acetone. The mass spectrum (a) exhibits a [M+H]+/[M*+H]+ ratio > 1, which represents a high quality matrix, and the following spectrum (b) a [M+H]+/[M*+H]+ ratio < 1 representing a matrix of lower quality. Figure 2S Comparison of the [M+H]+/[M*+H]+ (a) and [2M+H]+/[M*+H]+ (b) ratios of five various CHCA matrix batches (A, B, C, D and E, matrix solvent: acetone) obtained on a bench-top (MALDI IV) and floor-standing high resolution TOF instrument (AXIMA-CFR). Figure 3S Positive-ion MALDI FT-ICR mass spectrum of the matrix E (including highest amount of the contaminant) with the region around m/z 102. The spectrum was internally calibrated with following matrix signals: [M-CO2+H]+, [M-H2O+H]+ and [M+H]+. The RMS error on the three point calibration was -1.22 ppm. The mass spectrometric resolving power observed for the m/z 102.1276 signal was 230000 (FWHM). Figure 4S Positive-ion MALDI high energy (ELab 2 keV) CID (LinTOF/RTOF) mass spectrum of the precursor ion m/z 102.2 (derived from matrix E in acetone).

  3. Fig. 1S a [M+H]+ %Int. 190 100 90 [M-H2O+H]+ 80 172 70 60 50 [M*+H]+ 40 280 102 [2M+H]+ [M-CO2+Na]+ [M+Na]+ 30 168 212 379 20 10 0 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 Mass/Charge

  4. Fig. 1S b [M*+H]+ %Int. 102 100 90 80 70 60 50 40 [M-CO2+Na]+ [M+Na]+ [M+H]+ 30 190 172 [2M+H]+ 20 212 379 10 0 100 120 14 0 160 180 200 220 240 260 280 300 320 340 360 380 400 Mass/Charge

  5. Fig. 2S a

  6. Fig. 2S b

  7. Fig. 3S [M*+H]+ 102.1276 12C6H16N1 observed at m/z: 102.1276 Theoretical mass at m/z: 102.12772 Error: –1.2ppm m/z 102.1 102.2 102.3 102.4

  8. H H Fig. 4S Precursor ion C6H16N [M*+H]+ 58.14 600 Intensity 72.16 73.17 59.14 74.18 44.11 60.16 102.20 0 60 30 20 40 90 70 80 50 100 m/z

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