Method for detecting related substances in cinmetacin related product by high performance liquid chromatography
A related product, high-efficiency liquid phase technology, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as poor repeatability, low sensitivity, and poor specificity
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Embodiment 1
[0037] Choice of mobile phase
[0038] Choose acetic acid aqueous solution-acetonitrile, phosphate buffer saline-acetonitrile two mobile phase systems. When using the acetic acid aqueous solution-acetonitrile system, the components cannot be completely separated; in the phosphate buffer-acetonitrile system, due to the small concentration of the buffer salt selected, while ensuring good repeatability of the chromatographic peak retention time, the The damage to the chromatographic column is small, the peak shape is symmetrical, and the separation effect is good. Therefore, choose phosphate buffer - acetonitrile system as the mobile phase.
Embodiment 2
[0040] Establishment of methodology
[0041] 1. Specificity test
[0042] 1.1 Separation of the main starting materials, intermediates, degradation products and the main peak of Guimeixin for the synthesis of Guimeixin
[0043] Precisely measure 20 μl of the solution of cinnamexin, p-aminoanisole, sodium p-methylphenylhydrazine sulfonate, cinnamon hydrazine, and acid and alkali degradation products, inject it into the liquid chromatograph, record the chromatogram, and the spectrum shows that each component The degree of separation meets the requirements.
[0044] Table 1: The main starting materials, intermediates, degradation products and peak elution time of Guimeixin for the synthesis of Guimeixin
[0045]
[0046] 1.2 Acid, alkali, heat damage test
[0047] Acid destruction test solution: Accurately measure 10 mg of Guimeixin (batch number: 20150815), put it in a 50 ml measuring bottle, add 2.0 ml of 1.0 mol / L hydrochloric acid solution, let it stand for 2 hours, add...
Embodiment 3
[0066] Determination of related substances in Guimeixin finished products.
[0067] 1. Chromatographic conditions:
[0068] Column: Waters C18 (4.6 × 250mm, 5μm); detection wavelength 291nm; flow rate 1.0ml / min; Potassium oxide solution is adjusted to PH4.0);
[0069] The mobile phase adopts the gradient elution method, and the gradient elution is performed according to the following table:
[0070] Table 5: Gradient elution table
[0071]
[0072] 2. Preparation of relevant solutions and mobile phases:
[0073] 2.1 Preparation of relevant solutions
[0074] 2.1.1 Preparation of 20% potassium hydroxide solution
[0075] Weigh 20g of potassium hydroxide, add water to dissolve and dilute to 100ml.
[0076] 2.1.2 Preparation of 0.01mol / L potassium dihydrogen phosphate buffer solution
[0077] Weigh 1.3609 g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000 ml, and adjust the pH to 4.0 with 20% potassium hydroxide.
[0078] 2.1.3 Preparation ...
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