Method for preparing vasopressin deamidization impurities
A technology for deamidation and impurities, applied in the field of biopharmaceuticals, can solve the problems of dilute sample concentration, low yield and large volume, and achieve the effect of optimizing the production process
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[0029] Example 1
[0030] Example 1 (Detection of the crude product of vasopressin deamidation impurity precursor and the purity of the purified product solution by HPLC)
[0031] Instrument: Waters 2695 / 2489 High Performance Liquid Chromatograph
[0032] Separation column: Agilent XDB-C18 4.6×250mm, 5μm
[0033] Mobile phase: A is 0.1% TFA aqueous solution by volume, B is acetonitrile aqueous solution with 0.1% TFA-50% by volume (TFA is trifluoroacetic acid)
[0034] The flow rate is 1.0mL / min, the detection wavelength is 214nm, the room temperature detection, the elution gradient is shown in the table below, and the percentage is the volume percentage.
[0035] Elution step Elution time Eluent 1 0~5min 95%A+5%B 2 5~25min 95%A+5%B→50%A+50%B 3 25~30min100%B 4 30~35min 95%A+5%B
Example Embodiment
[0036] Example 2 (packing of 75mm inner diameter L&L4003 preparation column)
[0037] Using Load&Lock dynamic axial compression and static locking technology, the packing is styrene-divinylbenzene copolymer (reversed-phase packing Agilent PLRP-S), pore size 10nm, particle size 10μm, packing density 0.33g / mL, packed into the column Bed pressure 650psi, using Varian chromatographic packing system, 370g dry powder packing, 2L methanol after stirring and homogenizing, pour into 75mm inner diameter L&L4003 preparative column, compression ratio 3:1, carrier gas N 2 , Adjust the carrier gas pressure to make the oil pressure gauge pressure 2000psi, dynamic axial compression to the height of the column bed 26cm, as the preparation column for reversed-phase cyclization, reversed-phase purification and reversed-phase desalination.
Example Embodiment
[0038] Example 3 Reversed-phase cyclization, reversed-phase purification and reversed-phase desalination of crude raw material of vasopressin deamidation impurity precursor
[0039] Instrument: Varian SD-1 high pressure liquid preparation system
[0040] Chromatographic column: Example 2 self-installed preparative column Load&Lock4003 75×260mm, PLRP-S 10μm 10nm
[0041] The crude product of vasopressin deamidation impurity precursor is the crude product of vasopressin deamidation impurity precursor prepared by solid-phase synthesis through cracking and drying, and the structural formula is Cys-Tyr-Phe-Gln-Asn-Cys-Pro-Arg-Gly The trifluoroacetate.
[0042] The crude vasopressin deamidation impurity precursor solution is a 5 g / L solution formed by dissolving the above crude vasopressin deamidation impurity precursor in an acetonitrile aqueous solution with a concentration of 5% by volume.
[0043] The mobile phase A1 is purified water, and A2 is 0.03 volume percent H 2 O 2 NaOH aqueous s...
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