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1 1S SUPPORTING INFORMATION: The discovery of the once weekly glucagon like peptide 1 (GLP-1) analog semaglutide Jesper Lau*, Paw Bloch, Lauge Schäffer, Ingrid Pettersson, Jane Spetzler, Jacob Kofoed, Kjeld Madsen, Lotte Bjerre Knudsen, James McGuire, Dorte Bjerre Steensgaard, Holger Martin Strauss, Dorte X. Gram, Sanne Moller Knudsen, Flemming Seier Nielsen, Peter Thygesen, Steffen Reedtz-Runge and Thomas Kruse. Contents of supporting information: 2S - 8S: 9S 13S: Mass spectrometric methods and data. UPLC methods and data used for purity analysis.
2 2S Mass spectrometric methods and data. MALDI-TOF: Molecular weights of the peptides were determined using matrix-assisted laser desorption time of flight mass spectroscopy (MALDI-MS), recorded on a Microflex (Bruker). A matrix of alfa-cyano-4-hydroxy cinnamic acid was used. Or altenatively with electrospray ionization using the system stated in the scheme and according to the list below: Agilent TOF: An Agilent Technologies LC/MSD TOF (G1969A) mass spectrometer was used to identify the mass of the sample after elution from an Agilent 1200 series HPLC system. The de-convolution of the protein spectra was calculated with Agilent s protein confirmation software. Eluents: A: 0.1% Trifluoro acetic acid in water; B: 0.1% Trifluoro acetic acid in acetonitrile. Column: Zorbax 5u, 300SB-C3, 4.8x50mm. Gradient: 25% - 95 % B over 15 min. Sciex3000 A Perkin Elmer Sciex API 3000 mass spectrometer was used to identify the mass of the sample after elution from a Perkin Elmer Series 200 HPLC system. Eluents: A: 0.05% Trifluoro acetic acid in water; B: 0.05% Trifluoro acetic acid in acetonitrile. Column: Waters Xterra MS C-18 X 3 mm id 5 µm. Gradient: 5% - 90 % B over 7.5 min at 1.5ml/min LCT premier Performed on a setup consisting of Waters Acquity UPLC system and LCT Premier XE mass spectrometer from Micromass. Eluents: A: 0.1% Formic acid in water; B: 0.1% Formic acid in acetonitrile The analysis was performed at RT by injecting an appropriate volume of the sample (preferably 2-10µl) onto the column which was eluted with a gradient of A and B.The UPLC conditions, detector settings and mass spectrometer settings were: Column: Waters Acquity UPLC BEH, C-18, 1.7µm, 2.1mm x 50mm. Gradient: Linear 5% - 95% acetonitrile during 4.0 min (alternatively 8.0 min) at 0.4ml/min. Detection: 214 nm (analogue output from TUV (Tunable UV detector)) MS ionisation mode: API-ES; Scan: amu (alternatively amu), step 0.1 amu. Sciex 100 or 150 was performed on a setup consisting of Sciex API 100 (or150) Single quadropole mass spectrometer, Perkin Elmer Series 200 Quard pump,perkin Elmer Series 200 autosampler, Applied Biosystems 785A UV detector, Sedex 75 evaporative light scattering detector.the instrument control and data acquisition were done by the Sciex Sample control software running on a Windows 2000 computer. The HPLC pump is connected to two eluent reservoirs containing: A: 0.05% Trifluoro acetic acid in water B: 0.05% Trifluoro acetic acid in acetonitrile. The analysis is performed at room temperature by injecting an appropriate volume of the sample (preferably
3 3S 20 l) onto the column which is eluted with a gradient of acetonitrile.the HPLC conditions, detector settings and mass spectrometer settings used are giving in the following table.column: Waters Xterra MS C-18 X 3 mm id 5 um; Gradient: : 5% - 90 % acetonitrile linear during 7.5 min at 1.5ml/min;Detection : 210 nm (analogue output from DAD);ELS (analogue output from ELS), 40 C.MS ionisation mode API-ES.
4 4S Alalog # MS method Mol Weight Calc. (found) Ions found m/z GLP ,7 N/A liraglutide 3751,2 (3751) semaglutide 4113,6 (4113) ,7 (3384) Sciex ,3 (3779.5) (LCT Premier); , LCT premier ,1 (3652) 1826, ,1 (3680) ,6 (4099)
5 5S ,7 (3397) ,2 (3765) LCT premier ,4 (3926)) 1309,8. Sciex ,4 (3910) ,5 (4055) 1352, ,7 (4200) 1051,7 1401, ,6 (4083) , LCT premier ,4 (4029) ,5 (4056) ,4 (3956) 1319,8
6 6S ,5 (4086) ,2 (3693) ,3 (3824) ,4 (3968) ,6 (4113) ,6 (4112) MALDI-TOF 24 alpha-cyano-4- hydroxycinnamic acid 4258,7 (4256) ,8 (4248) ,7 (4242) ,8 (4372)
7 7S ,6 (4182) ,6 (4069) ,5 (4053) ,6 (4142) 1036,7 1381, ,7 (4169) ,4 (3970) ,4 (3970) 993,8 1987,2 35 Agilent TOF 4084,6 (4084.9)
8 8S 36 Agilent TOF 4114,6 ( ,5 (3938) MALDI-TOF alpha-cyano-4- hydroxycinnamic acid 4156,7 (4156.8) MALDI-TOF alpha-cyano-4- hydroxycinnamic acid 4142,7 (4141,9) 4141, ,2 (3694) 924,8 1232,4 1848, ,3 3851,1 1284,8 964, ,6 (4140,7) 829,5 1036, 1381, ,8 (4269) ,6 (4126,7) 1376,6
9 9S UPLC and HPLC methods used for purity analysis: General methods: The RP-HPLC analysis may be performed using UV detection at 214 nm and e.g. a Vydac 218TP54 4.6mm x 250mm 5 C-18 silica column (The Separations Group, Hesperia, USA) and eluted at e.g. 1 ml/min at 42 o C. Most often one of four different elution conditions are used: A1: Equilibration of the column with a buffer consisting of 0.1M (NH 4 ) 2 SO 4, which was adjusted to ph 2.5 with concentrated H 2 SO 4 and elution by a gradient of 0% to 60% CH 3 CN in the same buffer during 50 min. B1: Equilibration of the column with 0.1% TFA / H 2 O and elution by a gradient of 0% CH 3 CN / 0.1% TFA / H 2 O to 60% CH 3 CN / 0.1% TFA / H 2 O during 50 min. B6: Equilibration of the column with 0.1% TFA / H 2 O and elution by a gradient of 0% CH 3 CN / 0.1% TFA / H 2 O to 90% CH 3 CN / 0.1% TFA / H 2 O during 50 min. Alternatively the RP-HPLC analysis was performed using UV detection at 214 nm and a Symmetry300, 3.6mm x 150mm, 3.5 C-18 silica column (Waters) which was eluted at 1 ml/min at 42 o C. B4: Equilibration of the column with 0.05% TFA / H 2 O and elution by a gradient of 5% CH 3 CN / 0.05% TFA / H 2 O to 95% CH 3 CN / 0.05% TFA / H 2 O during 15 min.
10 10S Analytical methods, HPLC and UPLC Method name Eluent A Eluent B Linear gradient column Column temp C. Run time (min) Flow rate ml/min B4 acetonitrile 1% TFA in water 5-95% Symmetry300 C18, um, 3.9 mm x 150 mm RX acetonitrile 1% TFA in water 5-95% Symmetry300 C18, um, 3.9 mm x 250 mm J acetonitrile 1% TFA in water 20-65% Jupiter proteo C12, um, 4.6 mm x 250 mm B6 acetonitrile 0.1% TFA in water 0-90% Vydac 218TP54 4.6mm x -18 silica column % Acetonitrile, 0.05% Trifluoroacetic acid B % Acetonitrile, 0.05% Trifluoroacetic acid 07 20% Isopropanole, 20% Water and 60% Acetonitrile 99.95% Water, 0.05% Trifluoroacetic acid 99.95% Water, 0.05% Trifluoroacetic acid 0.09 M di-ammonium Hydrogen Phosphate (aq) and 10% Acetonitrile, ph % ACQUITY UPLC BEH C18, 1.7um, 2.1 mm x 150 mm column 5-60 BEH130, C18, 1.7um, 2.1x150mm Step gradient: 35% B over 2 minutes, then 35% to 65% B over 15 minutes, then 65% to 80% B over 3 minutes and finally 80% B over 1 minute Phenomenex Kinetex C18, 1.7um, 2.1 mm x 150 mm column A6 80%acetonitrile 10mM TRIS and 15mM ammonium sulphate ph 7.3 in 20%acetonitrile 80% water A3 70 % acetonitrile. A: 90 % H 2 O, 10 % CH 3 CN, 0.25 M ammonium bicarbonate; B: 70 % CH 3 CN, 30 % H 2 O HSS T3, 1.8um, 2.1 mm x 150 mm column HSS T3, 1.8um, 2.1 mm x 150 mm column
11 11S List of analytical data: Analog # Retention time Purity (min) (%) liraglutide B4 Method semaglutide B B J B B B B B A B B B B B B B B B A B B B B B B B B6
12 12S A B B4 A B4 A B B B B RX
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