Method for simultaneously detecting salicylic acid, aristolochic acid A, sodium cyclamate and beta-naphthol

A technology for aristolochic acid and salicylic acid, applied in the field of simultaneous detection of salicylic acid, aristolochic acid A, cyclamate and β-naphthol, which can solve the problems of simultaneous detection, insufficient detection sensitivity, and false peaks of body interference And other issues

Active Publication Date: 2013-09-11
JILIN TOBACCO IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, there are ion chromatography, gas chromatography, ultra-high performance liquid chromatography, etc. for the determination of the above four substances, but these methods have certain limitations, such as insufficient detection sensitivity and interference from the body. Phenomena such as large false peaks and inability to detect at the same time

Method used

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  • Method for simultaneously detecting salicylic acid, aristolochic acid A, sodium cyclamate and beta-naphthol
  • Method for simultaneously detecting salicylic acid, aristolochic acid A, sodium cyclamate and beta-naphthol
  • Method for simultaneously detecting salicylic acid, aristolochic acid A, sodium cyclamate and beta-naphthol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Weigh 0.0020g salicylic acid, 0.0020g aristolochic acid A, 0.0020g cyclamate and 0.0020g β-naphthol respectively, and dissolve them in ammonia solution-methanol with a volume ratio of 10:90 to 100mL. Concentration is 2mmol / L, and the molar concentration that obtains salicylic acid, aristolochic acid A, cyclamate and β-naphthol is the mixed stock solution of 20 μ g / mL;

[0090] Accurately pipette different volumes of the mixed stock solution and dilute it into a standard working solution with a molar concentration of 20ng / mL~1500ng / mL.

[0091] The obtained standard working solution is subjected to ultra-high performance liquid chromatography separation:

[0092] The column is ZORBAX Eclipse Plus C 18 (2.1mm×150mm, 1.8μm);

[0093] The flow rate is 0.25mL / min;

[0094] The column temperature is 30°C;

[0095] The injection volume is 5 μL;

[0096] Mobile phase A is an ammonia solution with a molar concentration of 2mmol / L, and mobile phase B is acetonitrile;

[0097]...

Embodiment 2

[0113] according to figure 1 The flow shown is to detect the tobacco additives, figure 1 Schematic flow chart of the method provided for the embodiment of the present invention:

[0114] Accurately weighed 1g of tobacco additive C10 purchased from a flavor and fragrance factory in Yanbian, according to sample solution preparation, chromatographic analysis conditions, and mass spectrometry detection conditions in the example 1, salicylic acid, aristolochic acid A, Cyclamate and β-naphthol are detected, according to the peak area of ​​salicylic acid, cyclamate, aristolochic acid A and β-naphthol chromatographic peak that obtains, and the salicylic acid that embodiment 1 obtains, cyclamate, equine The regression equation of A and β-naphthol calculates the mass concentration of salicylic acid, cyclamate, aristolochic acid A and β-naphthol in the solution to be tested; according to the obtained solution of salicylic acid , the mass concentration of cyclamate, aristolochic acid A ...

Embodiment 3

[0122] Accurately weigh 1g of tobacco additive C20 purchased from a flavor and fragrance factory in Yanbian, adopt the technical scheme of Example 2, detect the content of salicylic acid, aristolochic acid A, cyclamate or β-naphthol therein, the results are as follows As shown in Table 3, Table 3 is the test results obtained in Example 2 and Example 3 of the present invention.

[0123] Table 3 Test results obtained in Example 2 and Example 3 of the present invention.

[0124]

[0125] The detection limit of the method provided by the invention is respectively 8.0ng / g, 6.0ng / g, 10.0ng / g, 10.0ng / g to salicylic acid, aristolochic acid A, cyclamate and β-naphthol, at 20ng Good linearity in the range of / mL~1000ng / mL, correlation coefficient R 2 0.9991 or more. This shows that the method provided by the invention has high sensitivity and the obtained detection result is accurate.

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Abstract

The invention provides a method for simultaneously detecting salicylic acid, aristolochic acid A, sodium cyclamate and beta-naphthol. According to the method, in the extraction process, the interference of partial interference substances in a sample to be detected to the salicylic acid, the aristolochic acid A, the sodium cyclamate and the beta-naphthol is shielded; moreover, when mass spectrometric detection is carried out, the contents of the salicylic acid, the aristolochic acid A, the sodium cyclamate and the beta-naphthol in the sample to be detected are more accurately tested in an electro-spraying ionization anion and multi-reaction monitoring scanning mode through quantitative determination of second-level ion fragments. Besides, by utilizing the method provided by the invention, the detection on the salicylic acid, the aristolochic acid A, the sodium cyclamate and the beta-naphthol is simultaneously realized, the interference of similar compounds is eliminated, the accuracy and the reliability of the detected components are ensured, the detection sensitivity is high, the repeatability is good, and high accuracy and precision are achieved; the method is applicable to rapid quantitative screening and evaluation on the salicylic acid, the aristolochic acid A, the sodium cyclamate and the beta-naphthol in cigarette additives.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical testing of additives, in particular to a method for simultaneously detecting salicylic acid, aristolochic acid A, cyclamate and β-naphthol. Background technique [0002] Salicylic acid, also known as o-hydroxybenzoic acid, is an important fine chemical raw material. In the pharmaceutical industry, salicylic acid is a widely used disinfectant and antiseptic, and it is also a new favorite of skin care products. However, in my country, salicylic acid is prohibited from being used in food processing and production, because salicylic acid has a corrosive effect. People eat foods containing salicylic acid, which can stimulate the lining and mucous membrane of the esophagus and digestive tract, and can interact with the The protein reacts. Consuming a large amount can cause symptoms such as vomiting, abdominal pain, shortness of breath, acidosis, etc., which seriously affects people's heal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 刘金霞黄飞李宝志李河霖王超臧婉辰
Owner JILIN TOBACCO IND
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