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Method for separating benzoic acid, sorbic acid, salicylic acid and phenoxyethanol and analyzing contents of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol in toothpaste

A technology of phenoxyethanol and sorbic acid, which is applied in the separation and content analysis of salicylic acid and phenoxyethanol, and in the field of benzoic acid and sorbic acid in toothpaste, which can solve the problem of large interference in sample analysis and is not suitable for high-throughput analysis and analysis instruments Higher requirements and other problems, to achieve the effect of high inter-column reproducibility, low detection limit and good chromatographic peak shape

Active Publication Date: 2018-05-01
苏州市金茂日用化学品有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent (Application No. 201110168425.X) uses methanol and ammonium acetate as the mobile phase, and adopts three-wavelength channel isocratic elution to separate preservatives benzoic acid, sorbic acid, and salicylic acid. Although the analysis time of this patent is relatively short, it uses three Channel for analysis and detection has high requirements for analytical instruments and is not suitable for high-throughput analysis of multiple indicators in samples; Chinese patent (application number 201510484674.8) uses methanol, acetonitrile, water, and sodium dihydrogen phosphate as four solvents to form the mobile phase. Gradient elution at room temperature for 40 minutes to separate phenoxyethanol and benzoic acid in chemicals, although this method has a good detection limit, but this method uses four-phase mobile phase mixing for analysis, which interferes with the analysis of actual samples larger

Method used

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  • Method for separating benzoic acid, sorbic acid, salicylic acid and phenoxyethanol and analyzing contents of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol in toothpaste
  • Method for separating benzoic acid, sorbic acid, salicylic acid and phenoxyethanol and analyzing contents of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol in toothpaste
  • Method for separating benzoic acid, sorbic acid, salicylic acid and phenoxyethanol and analyzing contents of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol in toothpaste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] To confirm the precision of the determination of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol content by high performance liquid chromatography:

[0033] (1) The standard working curve drawing of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol;

[0034] Accurately weigh a certain amount of standard substances of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol, and prepare standard solutions with concentrations of 0.5, 5, 25, 50, 100, 200, and 500 μg / mL with 30% aqueous methanol . Concentrations from low to high are analyzed by high-performance liquid chromatography in turn, and the corresponding spectra are obtained, such as figure 1 shown.

[0035] (2) Utilize high-performance liquid chromatography to measure the peak area of ​​benzoic acid, sorbic acid, salicylic acid and phenoxyethanol, the mensuration of peak area can be obtained by the area integral between chromatographic peak and baseline, and peak area is as shown in T...

Embodiment 2

[0059] The content of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol is analyzed using the method of the present invention.

[0060] (1) Accurately weigh 0.5g of the toothpaste sample to be tested into a 50mL centrifuge tube, add 10ml of 30% methanol to dissolve, shake well, and dilute to 50mL;

[0061] (2) Ultrasonic 10min of solution in step (1), 4000rpm centrifugal 10 minutes, get the supernatant and filter with the organic phase filter membrane of 0.45 μm to obtain the toothpaste solution to be tested.

[0062] (3) Utilize the peak area of ​​benzoic acid, sorbic acid, salicylic acid and phenoxyethanol in the toothpaste sample measured by high performance liquid chromatography, compare the standard working curve that makes in Example 1, draw benzoic acid, benzoic acid, phenoxyethanol in the toothpaste sample Content of sorbic acid, salicylic acid and phenoxyethanol.

[0063] The measurement conditions are:

[0064] Chromatographic column: AcclaimTM 120 type ...

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Abstract

The invention relates to detection and analysis of a toothpaste preservative, and concretely relates to a method for separating benzoic acid, sorbic acid, salicylic acid and phenoxyethanol and analyzing contents of the benzoic acid, the sorbic acid, the salicylic acid and the phenoxyethanol in a toothpaste. The method comprises the following steps of (1) utilizing a high performance liquid chromatography for drawing a standard work curve of the benzoic acid, the sorbic acid, the salicylic acid and the phenoxyethanol; (2) weighing a toothpaste sample, using a methanol aqueous solution for dissolving, stirring and ultrasonically dissolving, and then sizing to obtain a sample solution; (3) after centrifuging the sample solution in the step (2), filtering a liquid supernatant through a microfiltration membrane to obtain a liquid to be tested; (4) using the high performance liquid chromatography for testing the liquid to be tested in the step (3), obtaining peak areas of the benzoic acid, the sorbic acid, the salicylic acid and the phenoxyethanol in the toothpaste sample, and obtaining the contents of the benzoic acid, the sorbic acid, the salicylic acid and the phenoxyethanol in the toothpaste sample through the standard work curve in the step (1). The method provided by the invention can be used for completely separating the benzoic acid, the sorbic acid, the salicylic acid and the phenoxyethanol, and has the characteristics of high column efficiency, good selectivity, good repeatability, wide linearity range, high detection limit, simplicity in operation, and the like.

Description

technical field [0001] The invention relates to the detection and analysis of toothpaste preservatives, in particular to a method for the separation and content analysis of benzoic acid, sorbic acid, salicylic acid and phenoxyethanol in toothpaste. Background technique [0002] In recent years, food safety issues have emerged in an endless stream, which has aroused widespread concern in the society. Subsequently, some scholars and public opinion turned their perspective to oral care products, and toothpaste, as a representative of oral care products, is related to personal safety issues. Therefore, the content and safety supervision of various additives in toothpaste are particularly important. Benzoic acid, sorbic acid, salicylic acid, and phenoxyethanol are used as preservatives and added to toothpaste to delay the growth of microorganisms or the corruption caused by chemical changes. [0003] Benzoic acid is a scaly or needle-like crystal with the smell of benzene or fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 陈健芬邓维孙东方李丹
Owner 苏州市金茂日用化学品有限公司
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