CN102928545A - Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops - Google Patents

Abstract

The invention discloses a method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops. The method is a reversed phase high-performance liquid chromatography utilizing pure BHT as a reference substance and methanol-water as a moving phase. Compared with the prior art, the method is easy, accurate and high in specificity.

Description

The content assaying method of BHT in a kind of pranoprofen eye drops

Technical field:

The present invention relates to the content assaying method of BHT in a kind of pranoprofen eye drops, belong to drug quality control technology field.

Background technology:

Pranoprofen (Pranoprofen), chemical name: (RS)-and 2-(10-hydrogen-9-Evil-1-naphthazine-6-yl) propionic acid, chemical structural formula:

Molecular formula: C ₁₅H ₁₃NO ₃, 255.27

Pranoprofen is the non-steroidal anti-inflammatory analgesics thing of welfide company (former Ji Fu Pharmaceutical Co., Ltd, the pharmacy of existing Mitsubishi) exploitation.Senju Pharma Co., Ltd is developed as eye drops with it, goes on the market in Japan in 1988.The symptomatic treatment that is used for clinically the inflammation of eye section such as blepharitis, conjunctivitis, keratitis, sclerotitis.

BHT, chemical name are 2,6-di-tert-butyl-4-methy phenol, by Bayer A.G's invention, are used as antioxidant in food processing, rubber plastic.

Molecular formula: C ₁₅H ₂₄O, 220.35

Oxidation reaction easily occurs in the main ingredient pranoprofen in the pranoprofen eye drops, generates oxidation product, thus add BHT as antioxidant to keep the stable of preparation, prolong its term of validity.

Summary of the invention:

The object of the present invention is to provide the content assaying method of BHT in a kind of pranoprofen eye drops, it is accurate, easy to measure.

The present invention is achieved through the following technical solutions: the content assaying method of BHT in the pranoprofen eye drops is take the BHT sterling as reference substance, the reversed-phased high performace liquid chromatographic take methanol-water as mobile phase.

It is further characterized in that concrete assay method step is:

(1) chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water (90: 10) (take the glacial acetic acid adjust pH as 5.2) is mobile phase; Flow velocity is 1.0ml/min; The detection wavelength is 275nm, and sample size is 20 μ L; Theoretical cam curve is calculated by pranoprofen and is not less than 2500;

(2) preparation of reference substance solution: accurate BHT reference substance is an amount of, also quantitatively is diluted to the solution of 50 μ g/ml with the methyl alcohol dissolving, in contrast product solution;

(3) preparation of need testing solution: precision measures sample 5ml and puts in the 10ml volumetric flask, adds mobile phase and is diluted to scale, shakes up, as need testing solution;

(4) measure: get respectively each 20 μ L of reference substance solution and need testing solution and inject high performance liquid chromatograph, the record peak area is pressed the content that external standard method is calculated BHT in the test sample.

Measure the content of BHT in the pranoprofen eye drops with the present invention, owing to adopting reversed phase liquid chromatography to detect, specificity is strong, thereby easy, accurate.

Description of drawings:

Fig. 1 is the chromatogram of reference substance solution of the present invention;

Fig. 2 is the chromatogram of sample solution of the present invention.

Specific implementation method:

Further set forth the present invention below by example, but do not place restrictions on the present invention.

Embodiment 1:

Instrument: the Japanese Shimadzu LC-10AT VP of company high performance liquid chromatograph; The SPD-10A UV-detector; And the HPLC chromatographic work station of analytical instrument outfit;

Chromatographic column: Kromasil 100-5C18 chromatographic column (250mm * 4.6mm);

Reference substance: BHT reference substance (detect through HPLC, purity is 99.1%);

Reagent: purified water, methyl alcohol (chromatographically pure), glacial acetic acid (chromatographically pure);

Chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water (90: 10) (take the glacial acetic acid adjust pH as 5.2) is mobile phase; Flow velocity is 1.0ml/min; The detection wavelength is 275nm, and sample size is 20 μ L; Theoretical cam curve is calculated by pranoprofen and is not less than 2500;

The preparation of reference substance solution: accurate BHT reference substance is an amount of, also quantitatively is diluted to the solution of 50 μ g/ml with the methyl alcohol dissolving, in contrast product solution;

The preparation of need testing solution: precision measures sample 5ml and puts in the 10ml volumetric flask, adds mobile phase and is diluted to scale, shakes up, as need testing solution;

Measure: get respectively each 20 μ L of reference substance solution and need testing solution and inject high performance liquid chromatograph, the record peak area is pressed the content that external standard method is calculated BHT in the test sample.

The retention time of BHT is 10.32min in the pranoprofen eye drops, and the content of BHT is respectively after measured in three batch samples: 0.03 ‰, 0.04 ‰, 0.04 ‰.

Below disclose the present invention with preferred embodiment, so it is not intended to limiting the invention, and all employings are equal to replaces or technical scheme that the equivalent transformation mode obtains, all drops within protection scope of the present invention.

Claims (2)

1. the content assaying method of BHT in the pranoprofen eye drops is characterized in that take the BHT sterling as reference substance the reversed-phased high performace liquid chromatographic take acetonitrile-water as mobile phase.

2. the content assaying method of BHT in the pranoprofen eye drops according to claim 1 is characterized in that concrete assay method step is:

(1) chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; The volume ratio of methyl alcohol and water is 90: 10, take the glacial acetic acid adjust pH as 5.2 as mobile phase; Flow velocity is 1.0ml/min; The detection wavelength is 245nm, and sample size is 20 μ L; Theoretical cam curve is calculated by pranoprofen and is not less than 2500;

(2) preparation of reference substance solution: accurate BHT reference substance is an amount of, also quantitatively is diluted to the solution of 50 μ g/ml with the methyl alcohol dissolving, in contrast product solution;

(3) preparation of need testing solution: precision measures sample 5ml and puts in the 10ml volumetric flask, adds mobile phase and is diluted to scale, shakes up, as need testing solution;

(4) measure: get respectively each 20 μ L of reference substance solution and need testing solution and inject high performance liquid chromatograph, the record peak area is pressed the content that external standard method is calculated BHT in the test sample.

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