Analysis and detection method of palbociclib intermediates and impurities in palbociclib intermediates
A technology for intermediate and mass analysis, applied in the direction of analyzing materials, measuring devices, material separation, etc., can solve problems such as the reduction of drug solubility, and achieve the effect of effective control
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Embodiment 1
[0088] Instruments and conditions:
[0089] Shimadzu LC-2010AHT high performance liquid chromatograph and Shimadzu LC-solution workstation; Octadecylsilane bonded silica gel column (Waters C18, 4.6mm×150mm×5μm); use 0.01M ammonium acetate buffer as mobile phase A (unadjusted pH value is 6.6), acetonitrile as mobile phase B, perform linear gradient elution according to the elution gradient table above The detection wavelength is 235nm; the column temperature of the column oven is 30°C; the flow rate of the mobile phase is 1.0ml / min; the injection volume of the liquid phase analysis is 20μl.
[0090] experiment procedure:
[0091] Preparation of impurity stock solution: take appropriate amount of PB-SM1, PB-SM2, PB-1A, PB-1, PB-2D, PB-2B and PB-2A reference substances, weigh them accurately, add dichloromethane to dissolve and make A solution containing 0.2mg of PB-SM1, 0.2mg of PB-SM2, 0.2mg of PB-1A, 0.2mg of PB-1, 0.2mg of PB-2D, 0.2mg of PB-2B and 0.2mg of PB-2A in each 1...
Embodiment 2
[0098] Instruments and conditions:
[0099] Shimadzu LC-2010AHT high performance liquid chromatograph and Shimadzu LC-solution workstation; Octadecylsilane bonded silica gel column (Waters C18, 4.6mm×150mm×5μm); use 0.01M ammonium acetate buffer as mobile phase A, acetonitrile as mobile phase B, perform linear gradient elution according to the above table; detection wavelength is 235nm; column temperature is 30°C ; The flow rate of the mobile phase is 0.9ml / min; the injection volume of the liquid phase analysis is 20μl.
[0100] experiment procedure:
[0101] Preparation of impurity stock solution: take appropriate amount of PB-SM1, PB-SM2, PB-1A, PB-1, PB-2D, PB-2B and PB-2A reference substances, weigh them accurately, add dichloromethane to dissolve and make A solution containing 0.2mg of PB-SM1, 0.2mg of PB-SM2, 0.2mg of PB-1A, 0.2mg of PB-1, 0.2mg of PB-2D, 0.2mg of PB-2B and 0.2mg of PB-2A in each 1ml solution, as Impurity stock solution.
[0102] Preparation of syst...
Embodiment 3
[0107] Instruments and conditions:
[0108] Shimadzu LC-2010AHT high performance liquid chromatograph and Shimadzu LC-solution workstation; Octadecylsilane bonded silica gel column (Waters C18, 4.6mm×150mm×5μm); use 0.01M ammonium acetate buffer as mobile phase A, acetonitrile as mobile phase B, perform linear gradient elution according to the above table; detection wavelength is 235nm; column temperature is 30°C ; The flow rate of the mobile phase is 1.1ml / min; the injection volume of the liquid phase analysis is 20μl.
[0109] experiment procedure:
[0110] Preparation of impurity stock solution: take appropriate amount of PB-SM1, PB-SM2, PB-1A, PB-1, PB-2D, PB-2B and PB-2A reference substances, weigh them accurately, add dichloromethane to dissolve and make A solution containing 0.2mg of PB-SM1, 0.2mg of PB-SM2, 0.2mg of PB-1A, 0.2mg of PB-1, 0.2mg of PB-2D, 0.2mg of PB-2B and 0.2mg of PB-2A in each 1ml solution, as Impurity stock solution.
[0111] Preparation of syst...
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