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Method for measuring preservative through hollow fiber film microextraction combining online derivatization-gas chromatography

A technology of gas chromatography and fiber membrane, which is applied in the field of preservative determination, can solve the problems of large consumption of organic solvents, cumbersome extraction steps, and long time consumption, and achieve less consumption of organic solvents, fewer extraction steps, and avoid cross-contamination Effect

Active Publication Date: 2018-11-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most pretreatment methods have defects such as cumbersome extraction steps, long time-consuming, high cost, and large consumption of organic solvents.

Method used

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  • Method for measuring preservative through hollow fiber film microextraction combining online derivatization-gas chromatography
  • Method for measuring preservative through hollow fiber film microextraction combining online derivatization-gas chromatography
  • Method for measuring preservative through hollow fiber film microextraction combining online derivatization-gas chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The selection of embodiment 1 derivatization reagent

[0028] The role of the derivatization reagent during the experiment is to derivatize the acidic substance into an ester substance that is easy for gas phase analysis under the high temperature inlet. Choosing the appropriate derivatization reagent is beneficial to improve the detection sensitivity. Depend on figure 1 It can be seen that the polysulfone membrane will not decompose at 300°C, but after adding TMAH (tetramethylammonium hydroxide), two peaks were observed around 20min and 25min, which may be due to the decomposition of the membrane. Adding TMSH (trimethylammonium hydroxide) Sulfur) and no obvious peak was observed. Therefore, TMSH was chosen as the derivatization reagent.

Embodiment 2

[0029] The selection of embodiment 2 acid concentration

[0030] During the experiment, by adjusting the acidity of the water-soluble sample, the target object is deionized, thereby reducing its solubility in the sample aqueous solution. The influence of the concentration of HCl (0.01, 0.1, 0.5, 1 and 1.5mol / L) in the sample solution on the extraction efficiency was investigated. Other experimental conditions were: the stirring speed was 300rpm, the temperature was 50℃, and the extraction time was 30min. The results showed that when the concentration of hydrochloric acid increased from 0 to 0.5mol / L, the extraction efficiencies of both sorbic acid and benzoic acid increased significantly. efficiency. However, when the acid concentration was further increased, the extraction efficiency did not increase, so the concentration of hydrochloric acid was selected as 0.5mol / L.

Embodiment 3

[0031] The selection of embodiment 3 stirring speed

[0032] Accelerating the stirring speed can improve the mass transfer process, accelerate the speed of the target substance entering the membrane, and improve the extraction efficiency, but too fast stirring will destroy the structure of the membrane and reduce the extraction efficiency. The extraction efficiency was investigated when the stirring speed was 100, 200, 300, 400, and 500rpm. Other experimental conditions were: the concentration of hydrochloric acid was 0.5mol / L, the temperature was 50°C, and the extraction time was 30min. The results showed that the extraction efficiency was the highest at 200rpm, so the stirring rate was selected at 200rpm.

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Abstract

The invention provides a method for measuring benzoic acid and sorbic acid through hollow fiber microextraction combining online derivatization-gas chromatography. The pre-treatment extraction steps are less, the enrichment coefficient is high, the cost is low, the using amount of organic solvents is low, the method has the very good sample purification capability, and meanwhile, has the higher anti-matrix interference ability. In addition, the hollow fiber is low in cost, can be used disposably, and cross contamination among samples can be avoided.

Description

(1) Technical field [0001] The invention relates to a method for measuring preservatives, in particular to a method for measuring the content of benzoic acid and sorbic acid preservatives in food by combining hollow fiber membrane microextraction with on-line derivatization-gas chromatography. (2) Background technology [0002] Benzoic acid and sorbic acid are common preservatives, which can inhibit the growth and reproduction of bacteria and are widely used in the food industry. However, eating foods containing excessive amounts of benzoic acid and sorbic acid will affect the body’s absorption of vitamins and calcium, and aggravate human health. Liver burden, and cause toxic reaction or induce cancer. FAO and WHO have specified in detail the scope and dosage of benzoic acid and sorbic acid in different foods. my country also has strict regulations on the use of preservatives. The state stipulates the hygienic standards for the use of food additives (GB2760-2007 "Hygienic St...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 黄忠平黄小丽王丽丽刘会君李国华
Owner ZHEJIANG UNIV OF TECH
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