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Improved method for measuring content of patulin in beverage based on high performance liquid chromatography

A high-performance liquid chromatography, patulin technology, applied in the field of patulin detection, can solve the problems of affecting the accuracy of the results, the sample cannot be effectively separated, and the recovery rate of patulin is high, and the effect of reducing the interference of impurities is achieved.

Pending Publication Date: 2022-04-19
TIANDI YIHAO BEVERAGE JIANGMEN CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing method is optimized based on the second method of GB 5009.185-2016 "National Food Safety Standard for the Determination of Patulin in Food". At present, due to the relatively expensive price of patulin solid-phase purification column, a purification column can only be used once, and the detection cost Second, because the content of patulin is at trace levels, a small amount of impurities may cause the test results to deviate from the true value, and the purification column does not adsorb some impurity components, so that the final sample cannot be used in high performance liquid phase. For effective separation, the recovery rate of patulin is too high due to the influence of impurities, which affects the accuracy of the results

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  • Improved method for measuring content of patulin in beverage based on high performance liquid chromatography

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Embodiment 1

[0030] A method of improving the content of patulin in beverages based on high performance liquid chromatography, comprising the following steps:

[0031] 1) Weigh 25.0mL sample into a 50mL centrifuge tube, then add 2mL potassium ferrocyanide and 2mL zinc acetate, add water to 50mL, vortex for 5min and mix well;

[0032] 2) Then centrifuge at 4000r / min for 5min, draw 25mL of the supernatant into another 50mL centrifuge tube, add 1g of activated carbon to absorb impurities, then add acetonitrile to 50mL, vortex for 5min, then centrifuge at 4000r / min for 5min , to obtain the supernatant to be purified.

[0033] 3) Aspirate 10 mL of the supernatant obtained in step 2), evaporate to nearly dryness using a vacuum rotary evaporator at 40° C., dissolve with 4% acetic acid solution and set the volume to 2 mL to obtain the detection solution to be inserted into the needle;

[0034] 4) chromatographic detection and ultraviolet detection are carried out to the detection solution of step...

Embodiment 2

[0044] A method of improving the content of patulin in beverages based on high performance liquid chromatography, comprising the following steps:

[0045] 1) Weigh 25.0mL sample into a 50mL centrifuge tube, add 2.5mL potassium ferrocyanide and 2.5mL zinc acetate, add water to 50mL, vortex for 5 minutes and mix well;

[0046] 2) Then centrifuge at 5000r / min for 3min, draw 25mL of the supernatant into another 50mL centrifuge tube, add 0.8g of activated carbon to absorb impurities, then add acetonitrile to 50mL, vortex for 5min and then centrifuge at 5000r / min 3min to obtain the supernatant to be purified.

[0047] 3) Aspirate 10 mL of the supernatant obtained in step 2), evaporate to nearly dryness using a vacuum rotary evaporator at 50° C., dissolve with 5% acetic acid solution and set the volume to 2 mL to obtain the detection solution to be inserted into the needle;

[0048] 4) Perform chromatographic detection and ultraviolet detection on the detection solution obtained in ...

Embodiment 3

[0058] A method of improving the content of patulin in beverages based on high performance liquid chromatography, comprising the following steps:

[0059] 1) Weigh 25.0mL sample into a 50mL centrifuge tube, add 1.7mL potassium ferrocyanide and 1.7mL zinc acetate, add water to 50mL, vortex for 5 minutes and mix well;

[0060] 2) Then centrifuge at 5000r / min for 3min, draw 25mL of the supernatant into another 50mL centrifuge tube, add 0.96g of activated carbon to absorb impurities, then add acetonitrile to 50mL, vortex for 5min and centrifuge at 4500r / min 3min to obtain the supernatant to be purified.

[0061] 3) Aspirate 10 mL of the supernatant obtained in step 2), evaporate to nearly dryness using a vacuum rotary evaporator at 40° C., dissolve with 5% acetic acid solution and set the volume to 2 mL to obtain the detection solution to be inserted into the needle;

[0062]4) Perform chromatographic detection and ultraviolet detection on the detection solution obtained in step ...

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Abstract

The invention discloses an improved method for measuring the content of patulin in a beverage based on a high performance liquid chromatography, which comprises the following steps of: limiting a pretreatment step before sample detection: firstly adsorbing protein components in the beverage by using potassium ferrocyanide and a zinc acetate solution, and then adsorbing components such as pigments in the beverage by using activated carbon; after purification, patulin in a beverage sample is subjected to chromatographic detection and ultraviolet detection, so that poison spreading mildew in the beverage can be effectively separated, a purer sample can be obtained, and interference of impurities can be reduced.

Description

technical field [0001] The invention relates to the technical field of patulin detection, in particular to an improved method for determining the content of patulin in beverages based on high performance liquid chromatography. Background technique [0002] Patulin, also known as patulin, is a secondary metabolite produced by the metabolism of various fungi in the genus Aspergillus, Penicillium, and Filamentosa. Initially, patulin was reported in the literature as a potential broad-spectrum antibiotic capable of inhibiting more than 75 different bacterial species. However, subsequent studies have found that patulin not only inhibits bacteria, but also exhibits certain toxicity to fungi, higher plants, and animals. Patulin is a mycotoxin that has serious harm to the human body and can cause a variety of toxicity in the body, including acute toxicity, chronic toxicity and cytotoxicity. In view of the toxicity of patulin, many countries and regions have imposed limit standards...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 冯雪红蔡伟源邹清辉罗培余
Owner TIANDI YIHAO BEVERAGE JIANGMEN CITY