Method for testing exenatide and impurities thereof by using high performance liquid chromatography
A technology of high-performance liquid chromatography and exenatide, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that peaks cannot be separated or the resolution cannot meet the requirements, and the specificity is poor, so as to achieve good durability and detection Low cost and simple preparation
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Embodiment 1
[0017] Example 1 The establishment process of the inventive method:
[0018] 1. Instruments and reagents
[0019] Instruments: Waters 2489 detector, Waters e2695 pump, Empower chromatography workstation;
[0020] Reagents: acetonitrile (chromatographically pure); sodium heptanesulfonate, sodium pentanesulfonate, sodium hexanesulfonate, sodium octanesulfonate, sodium nonanesulfonate, sodium decanesulfonate, trifluoroacetic acid, phosphoric acid ( Analytical pure); water for injection.
[0021] 2. Establishment of Exenatide Impurity Determination Method
[0022] (1) Selection of wavelength: Exenatide and its impurities (Exenatide fragment3-39, Acetyl Exenatide, L-Glu 13 Exenatide, D-Ser 8 Exenatide, D-Ser 11 Exenatide, Met[O] Exenatide, D-His 1 Exenatide, Des-Gly 2 Exenatide) UV absorption has its own characteristics. We measured its absorption spectrum in 25% acetonitrile solution under ultraviolet light. Exenatide and its impurities all have strong ultrav...
Embodiment 2
[0052] Example 2 Determined according to high performance liquid chromatography (Chinese Pharmacopoeia 2010 edition two appendix VA).
[0053] Determination of various impurities of exenatide: use octylsilane bonded silica gel as filler, acetonitrile-sodium heptanesulfonate solution (1.2mmol / L sodium heptanesulfonate solution, adjust pH to 4.0 with phosphoric acid) (10 :90) was mobile phase A, acetonitrile-sodium heptanesulfonate solution (52:48) was mobile phase B, and gradient elution was carried out according to Table 2 below.
[0054]
[0055] The detection wavelength is 214nm; the flow rate is 1.2ml / min; the temperature of the autosampler is 6°C; the column temperature is 40°C, and the separation of the main peak and miscellaneous peaks should meet the requirements.
[0056] Preparation of exenatide test solution: Take an appropriate amount of exenatide sample (about 10 mg of exenatide), weigh it accurately, and prepare it with 25% acetonitrile so that the concentrat...
Embodiment 3
[0059] Example 3 Determined according to high performance liquid chromatography (Chinese Pharmacopoeia 2010 edition two appendix VA).
[0060] Determination of various impurities of exenatide: use octylsilane bonded silica gel as filler, acetonitrile-sodium heptanesulfonate solution (1.8mmol / L sodium heptanesulfonate solution, adjust pH to 4.8 with phosphoric acid) (10 :90) was mobile phase A, acetonitrile-sodium heptanesulfonate solution (52:48) was mobile phase B, and gradient elution was carried out according to Table 4 below.
[0061]
[0062] The detection wavelength is 214nm; the flow rate is 1.2ml / min; the temperature of the autosampler is 6°C; the column temperature is 40°C, and the separation of the main peak and miscellaneous peaks should meet the requirements.
[0063] Preparation of Exenatide Impurity Test Solution: Take an appropriate amount of exenatide sample (about 10 mg exenatide), accurately weighed, and prepare a concentration of about 1 ml of exenatide...
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