Content of miconazole nitrate and chlorhexidine gluconate in compound shampoo detection method
A technology of chlorhexidine gluconate and miconazole nitrate, which is applied in the field of content detection of miconazole nitrate and chlorhexidine gluconate in compound shampoos, can solve the problem of low response value and inapplicability of miconazole nitrate and gluconic acid The content determination of chlorhexidine, slow elution peak time and other problems, achieve high response value, improve detection efficiency, and solve the effect of content determination
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Embodiment 1
[0037] A kind of content detection method of miconazole nitrate and chlorhexidine gluconate in compound shampoo, comprises the following steps:
[0038] 1) Accurately weigh 1 g of compound miconazole nitrate shampoo, and prepare 200 mL of the test solution with a solvent, wherein the content of miconazole nitrate is about 0.1 mg / mL, and the content of chlorhexidine gluconate is about 0.1 mg / mL ; The solvent is composed of acetonitrile, 0.05mol / L disodium hydrogen phosphate solution and triethylamine in a volume ratio of 45:55:1, and the pH value is adjusted to 3.0 with phosphoric acid solution.
[0039] 2) Get 10 μ L of the test solution, inject it into a high-performance liquid chromatograph for detection, and obtain the following: figure 1 In the chromatogram shown, peak 1 corresponds to miconazole nitrate, and peak 2 corresponds to chlorhexidine gluconate.
[0040] The chromatographic conditions are:
[0041] Chromatographic column: ZORBZX Eclipse XDB-C18Analytical 4.6×15...
Embodiment 2
[0049] Embodiment 2 system suitability verification
[0050] Chromatographic conditions: a chromatographic column using octadecylsilane bonded silica gel as a filler; the mobile phase is composed of acetonitrile-0.05mol / L disodium hydrogen phosphate solution-triethylamine in a volume ratio of 45:55:1, with phosphoric acid Adjust the pH to 3.0; the column temperature is 30°C, the flow rate is 1.0mL / min, and the detection wavelength is 230nm. The number of theoretical plates by miconazole nitrate and chlorhexidine gluconate should be greater than 2000, and the degree of separation should be greater than 1.5.
[0051] It has been verified by experiments that the theoretical plate numbers of miconazole nitrate and chlorhexidine gluconate are both greater than 2000, and the resolution is greater than 1.5, indicating that the system has good applicability.
Embodiment 3
[0052] Embodiment 3 specificity test
[0053] Precisely measure 10 μL of the diluent (methanol) and inject it into the liquid chromatograph, record the spectrum, and obtain a blank spectrum.
[0054] The reference substance of miconazole nitrate plus mobile phase is made into a solution containing about 0.1mg miconazole nitrate in every 1mL, and 10 μ L is precisely measured and injected into a liquid chromatograph, carried out according to the chromatographic conditions of Example 1, and the chromatogram is recorded. Obtain the chromatogram of reference substance (with reference to figure 1 ), it is known from the chromatogram that the retention time of miconazole nitrate is about 2.79min.
[0055] The chlorhexidine gluconate reference substance plus mobile phase is made into a solution containing about 0.1mg chlorhexidine gluconate in every 1mL, and precision measures 10 μ L and injects it into a liquid chromatograph, carries out according to the chromatographic conditions o...
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