Method for determining content of mythyl p-hydroxybenzoate and sodium benzoate in solution

A technology of methyl hydroxybenzoate and sodium benzoate, applied in the field of chemical inspection, can solve the problems of increased workload of inspection personnel in the deployment and use of analytical instruments, cumbersome inspection methods, passive work arrangements, etc., and achieves easy operation, good stability, and economical efficiency. effect of personnel

CN104297357AActive Publication Date: 2015-01-21SHANGHAI JINGFENG PHARMA
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2015-01-21

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Abstract

The invention relates to a method for determining content of mythyl p-hydroxybenzoate and sodium benzoate in a solution. The method is characterized in that a high performance liquid chromatography is adopted, and chromatographic conditions are adaptive to a system: octadecyl bonded silane is used as a filling agent and 1% acetonitrile-acetic acid is used as a mobile phase, wherein a volume ratio of a water phase to an organic phase is 72-70:28-30; a detection wavelength is 230 nm; a flow velocity is 0.6-1.0 ml per minute; a column temperature is 30+ / -5 DEG C; a number of theoretical plates is not smaller than 3,000 in terms of sodium benzoate; and a degree of separation is larger than 2.0. The method comprises the steps of precisely measuring a proper amount of a drug preparation solution; adding a mobile phase to dilute the solution into a test liquid with required concentration; shaking uniformly; injecting 10 [mu]L of the sample in a liquid chromatograph; recording a chromatogram; measuring methyl 4-hydroxybenzoate and sodium benzoate as reference substances; determining by using the same method; and calculating according to peak area by using an external standard method. With the method, quantitative analysis of methyl 4-hydroxybenzoate and sodium benzoate can be completed under the same chromatographic conditions; the determination method is simple and practicable; and the determined indexes are accurate.
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Description

Technical field:

[0001] The invention relates to the field of chemical testing and the technical field of drug analysis, in particular to a method for determining the content of methyl p-hydroxybenzoate and sodium benzoate in a solution. Background technique:

[0002] An existing pharmaceutical preparation contains two preservative ingredients: methyl p-hydroxybenzoate and sodium benzoate. At present, there is no analytical method for simultaneous detection of both under the same chromatographic conditions.

[0003] Methyl p-hydroxybenzoate, also known as methyl paraben, has a strong antibacterial effect, and it has an ideal effect on preventing fermentation and mildew of the preparation when used in combination with sodium benzoate.

[0004] At present, the detection methods of these two preservatives can only be tested for the content of a single methyl p-hydroxybenzoate and sodium benzoate. If the content determination of the two components is carried out separately, the ...

Examples

Embodiment 1

[0022] According to the "Chinese Pharmacopoeia" 2010 edition two appendix VD high performance liquid chromatography determination.

[0023] Experimental method and process:

[0024] 1. Instruments and reagents

[0025] Chromatograph: 1260 high performance liquid chromatograph (manufacturer: Agilent)

[0026] Analytical balance: AG285 type (manufacturer: Mettler)

[0027] Test product: a drug preparation to be tested, known to contain 0.5 mg / ml of methyl p-hydroxybenzoate and 1 mg / ml of sodium benzoate.

[0028] 2. Chromatographic conditions and system adaptability

[0029] Chromatographic column Shim-pack VP-ODS C18 column (4.6mm×250mm, 5μm); with 1% acetic acid-acetonitrile as the mobile phase, the volume ratio of the aqueous phase to the organic phase is 70:30, the detection wavelength is 230nm, and the flow rate is 1.0ml per minute, the column temperature is 30°C, the number of theoretical plates is not less than 3000 based on sodium benzoate, and the resolution should ...