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Detection method of Jianer Qingqing solution

A detection method and a technology for clearing solution, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of lack of specific detection methods for free hydrogen cyanide

Pending Publication Date: 2021-12-31
云南省食品药品监督检验研究院
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  • Abstract
  • Description
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Problems solved by technology

[0003] Through the analysis of the traditional Chinese medicine preparations containing bitter almonds recorded in the "Chinese Pharmacopoeia", the steam distillation method is mainly to extract the mandelonitrile solution, and the content detection item of mandelonitrile is established in the quality standard of the preparation. At the same time, mandelonitrile is very easy to decompose As volatile free hydrogen cyanide, there is a safety risk, but free hydrogen cyanide lacks a specific and sensitive detection method

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  • Detection method of Jianer Qingqing solution
  • Detection method of Jianer Qingqing solution
  • Detection method of Jianer Qingqing solution

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preparation example Construction

[0073] In the present invention, the preparation method of described reference substance solution preferably comprises:

[0074] Dilute the standard substance for cyanogen component analysis in water with sodium hydroxide solution, add sodium chloride, and acidify with phosphoric acid solution.

[0075] In the present invention, the sodium hydroxide solution is preferably an aqueous sodium hydroxide solution; the concentration of the sodium hydroxide solution is preferably 0.08 to 0.12 mol / L, more preferably 0.09 to 0.11 mol / L, most preferably 0.1 mol / L.

[0076] In the present invention, the content of cyanate in the diluted water cyanide component analysis standard substance is preferably 20-30 μg / mL, more preferably 23-27 μg / mL, and most preferably 25 μg / mL.

[0077] In the present invention, the phosphoric acid solution is preferably an aqueous phosphoric acid solution; the volume concentration of the phosphoric acid solution is preferably 5-12%, more preferably 6-11%, m...

Embodiment 1

[0107] The stability of embodiment 1 mandelonitrile in solvent

[0108] Adopt high performance liquid chromatography to detect mandelonitrile solution:

[0109] Chromatographic conditions: Shimadzu LC-2040 high performance liquid chromatography, Agilent TC-C18 high performance liquid chromatography column (4.6mm×250mm, 5μm); mobile phase is acetonitrile-0.1% phosphoric acid solution (23:77), column flow 1mL / min; detection wavelength: 207nm; column temperature: 30°C; injection volume: 10μL.

[0110] Mandelonitrile reference substance (Shanghai Aladdin Biochemical Technology Co., Ltd., number M158766, batch number B2019085, marked purity 97.067%).

[0111] Method: Take an appropriate amount of mandelonitrile reference substance, and dissolve them with methanol, ethanol, acetonitrile, water, phosphoric acid aqueous solution with pH 1.5-6.0, 0.1%-1.0% (v / v) glacial acetic acid acetonitrile solution, and make each 1 mL of mandelonitrile-containing About 200 μg of the solution was...

Embodiment 2

[0121] Determination of Mandelonitrile in Jianer Qingjie Solution by HPLC

[0122] Instrument: Shimadzu LC-2040 high performance liquid chromatography.

[0123] The preparation of reference substance solution: get mandelonitrile reference substance (Shanghai Aladdin Biochemical Technology Co., Ltd., number M158766, lot number B2019085, marked purity 97.067%), accurately weighed, add the phosphoric acid aqueous solution that pH value is 2.5, gradually dilute, Prepare a serial concentration reference solution containing 1.033 μg, 5.164 μg, 10.328 μg, 24.432 μg, 48.864 μg, 103.279 μg, 147.493 μg, 198.599 μg, 244.318 μg, 294.987 μg of mandelonitrile respectively per 1 mL.

[0124] Preparation of the test solution: take an appropriate amount of Jianerqing solution sample, filter it with a 0.45 μm microporous membrane, and take the subsequent filtrate to obtain the product.

[0125] Preparation of negative control solution: According to the prescription preparation method contained...

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Abstract

The invention provides a detection method of a Jianer Qingqing solution. The detection method comprises the following step: detecting the mass content of mandelonitrile in the Jianer Qingqing solution by adopting high-phase liquid chromatography. In the detection process of the high-phase liquid chromatography, a solvent in a mandelonitrile reference substance solution is a glacial acetic acid acetonitrile solution or a phosphoric acid aqueous solution. From the basic consensus of poor stability of the mandelonitrile, the problem of poor stability of the mandelonitrile in a common solvent is solved, and the method suitable for determining the content of the mandelonitrile in the Jianer Qing solution is developed; and the real content composition of the free hydrogen cyanide and the mandelonitrile in a sample is obtained through respective detection of the free hydrogen cyanide and the mandelonitrile, so that the blank of quality control of the Jianer Qing solution at present can be filled, data with distinction degree can be provided for subsequent production process optimization and evaluation of safety, effectiveness and the like, and a thought is provided for quality control of the traditional Chinese medicine preparation containing the bitter apricot kernel aromatic water.

Description

technical field [0001] The invention belongs to the technical field of Jianer Qingjie liquid, and in particular relates to a detection method of Jianer Qingjie liquid. Background technique [0002] Jianer Qingjie Liquid is a Chinese patent medicine for pediatrics. It is made by extracting six medicinal materials such as bitter almonds. Epigastric fullness embolism. The bitter almonds in the prescription are added to the preparation after distillation to extract the aromatic water. The amygdalin in bitter almonds can be hydrolyzed to glucose and prunin under the catalysis of enzymes under conditions such as dampness and decoction, and prunin continues to be hydrolyzed to glucose and mandelonitrile (also known as amygdalin). Nitrile is extremely unstable and easily decomposes when heated to generate benzaldehyde and highly toxic hydrogen cyanide. Use gas chromatography-mass spectrometry to detect the volatile oil extracted from bitter almonds through steam distillation, whi...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 张元杰周兰郝文梅李哲媛来国防任杰红范兵
Owner 云南省食品药品监督检验研究院
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