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Novel sampling method applied to infrared spectroscopic analysis technique

A technology of infrared spectroscopy and infrared spectroscopy, which is applied in the field of new sample preparation for quantitative analysis of active ingredients in pharmaceutical preparations, can solve the problems of limited dosage forms of pharmaceutical preparations, inability to accurately weigh samples, uneven mixing of samples and KBr, etc. , to achieve the effect of expanding the scope of application, improving accuracy and reproducibility

Inactive Publication Date: 2016-10-12
SHENYANG POLYTECHNIC UNIV
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AI Technical Summary

Problems solved by technology

[0007] In order to solve the defects such as the inability to accurately weigh the sample quality in the traditional sample preparation process, the uneven mixing of the sample and KBr, the limitation of the dosage form of the measurement pharmaceutical preparation, and the inability to avoid the interference of excipients, etc., the present invention proposes a method for quantitative analysis of quinolones using infrared spectroscopic analysis technology. The new sample preparation method of drug-like preparations can add samples accurately and quantitatively with less consumption; it can significantly improve the precision of the measurement results; it can also accurately determine the accurate determination of dosage forms that cannot be handled by traditional methods; at the same time, it effectively eliminates the excipients interference with the assay

Method used

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  • Novel sampling method applied to infrared spectroscopic analysis technique
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  • Novel sampling method applied to infrared spectroscopic analysis technique

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Experimental program
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Effect test

preparation example Construction

[0053] (4) Preparation of standard samples and samples to be tested

[0054] Take 40.0 μL, 80.0 μL, 120.0 μL, 160.0 μL and 200.0 μL of the standard sample solution and inject them into 0.1000 g KBr matrix, dry at 100°C for 1 hour, grind and sieve to obtain a concentration of 2.0, 4.0, 6.0, 8.0, 10.0 mg / g standard sample;

[0055] Inject 120.0 μL of the solution to be tested into 0.1000 g of KBr matrix, dry at 100°C for 1 hour, remove the solvent water, then cool, grind, and sieve to obtain the sample to be tested;

[0056] (5) Determination by diffuse reflectance infrared spectroscopy

[0057]Place the sieved powder sample in the sample cup, scrape the surface, and scan its infrared spectrum by diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS); use a computer (IRsolution software) to process the data and obtain the analysis results;

[0058] (6) Compared with traditional methods

[0059] The measurement results were compared with the standard method to e...

Embodiment 1

[0062] Embodiment 1: Norfloxacin pharmaceutical preparation

[0063] (1) Experimental conditions

[0064] Solvent: 0.1mol / LHCl, drying temperature: 100°C, drying time: 1h,

[0065] (2) Instrument working conditions

[0066] Scanning wave number range: 400~4000cm -1 ; Scanning background: KBr (spectral pure); Resolution: 8.0cm -1 ; Number of scans: 30 times.

[0067] (3) Standard method for comparison: high performance liquid chromatography

[0068] (4) Selection of standard substance: norfloxacin; concentration of standard solution: 0.5 μg / μL; linear range of standard working curve: 0.2-1.0 mg / g; sampling volume of sample to be tested: 120.0 μL.

[0069] (5) The measurement results are shown in Table 1.

[0070] Table 1

[0071]

Embodiment 2

[0072] Embodiment 2: enoxacin pharmaceutical preparation

[0073] (1) Experimental conditions

[0074] Solvent: 0.1mol / LHCl, drying temperature: 100°C, drying time: 1h,

[0075] (2) Instrument working conditions

[0076] Scanning wave number range: 400~4000cm -1 ; Scanning background: KBr (spectral pure); Resolution: 8.0cm -1 ; Number of scans: 30 times.

[0077] (3) Standard method for comparison: ultraviolet spectrophotometry (UV)

[0078] (4) Selection of standard substance: enoxacin; concentration of standard solution: 0.5 μg / μL; linear range of standard working curve: 0.2-1.0 mg / g; sampling volume of sample to be tested: 120.0 μL.

[0079] (5) The measurement results are shown in Table 2.

[0080] Table 2

[0081]

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Abstract

The invention provides a novel sampling method applied to a diffuse reflection infrared spectroscopic analysis technique, and particularly discloses a novel sampling method applied to quantitative analysis of quinolone drug preparations through the diffuse reflection infrared spectroscopic analysis technique. The content of effective ingredients of different dosage forms such as drug tablets including norfloxacin, enoxacin, ofloxacin and the like, capsules and extracts is accurately measured by adopting the diffuse reflection infrared spectroscopic analysis technique. The defects of the traditional sampling process are overcome, the mass of a collected sample is accurately controlled according to the volume of a solution added into KBr, the sample and a diluant are mixed to be uniform, accurate measuring is achieved, and auxiliary material interference is effectively avoided.

Description

technical field [0001] The invention provides a novel sample preparation method applied to infrared spectrum analysis technology, especially capable of quantitatively analyzing active ingredients in pharmaceutical preparations. Background technique [0002] Infrared spectroscopy can be used not only for qualitative analysis of molecular composition and structure, but also for quantitative analysis of sample content. With the application of new Fourier transform infrared spectrometers and high-performance accessories and detectors, infrared spectroscopy is widely used in the field of quantitative analysis. Compared with other conventional detection methods, this method has simple sample preparation and does not require complicated sample preparation. Advanced pretreatment, fast analysis speed, low consumption of reagents and samples, basically no waste liquid, can realize non-destructive and non-polluting green analysis, wide application range, and accurate results. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/3563G01N21/3577G01N1/28
CPCG01N21/3563G01N1/28G01N21/3577G01N2021/3572
Inventor 张进吴心雨万瑞英刘利
Owner SHENYANG POLYTECHNIC UNIV
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