Method for rapidly measuring content of bongkrekic acid in food by automatic solid phase extraction-ultra performance liquid chromatography

A technology of ultra-high performance liquid phase and rice yeast acid, which is applied in the field of food safety testing, can solve the problems of short processing cycle, achieve high recovery rate, short pre-processing cycle, and reduce labor costs

Pending Publication Date: 2018-06-22
ZHEJIANG INST FOR FOOD & DRUG CONTROL
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AI Technical Summary

Problems solved by technology

[0005] For the deficiencies in existing rice yeast acid detection, the object of the present invention is to provide a kind of mixed anion automatic solid phase extraction-ultra-high performance liquid chromatography method for quickly measuring the method for rice yeast acid content in food, the pretreatment cycle of the method Short, low consumption of organic reagents, less environmental pollution, high recovery rate and sensitivity, easy operation, good repeatability, suitable for the determination of rice yeast acid in various food matrices, in addition, this experiment uses a secondary array detector, through Retention time and spectral scanning qualitative can realize the elimination and confirmation of false positive samples. Compared with mass spectrometry, the interference of matrix effect is eliminated, making the results accurate and reliable

Method used

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  • Method for rapidly measuring content of bongkrekic acid in food by automatic solid phase extraction-ultra performance liquid chromatography
  • Method for rapidly measuring content of bongkrekic acid in food by automatic solid phase extraction-ultra performance liquid chromatography
  • Method for rapidly measuring content of bongkrekic acid in food by automatic solid phase extraction-ultra performance liquid chromatography

Examples

Experimental program
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Effect test

Embodiment 1-10

[0040] Embodiment 1-10: Determination of the rice yeast acid content in dry corn

[0041] 1) After crushing 10 batches of dry cornmeal purchased in the market, weigh 20 g and place them in a conical flask, add 40 mL of 2 % ammonia water and 80 % acetonitrile aqueous solution as the extraction solvent, mix well, and soak for 1 h at room temperature in the dark. Place in an ultrasonic oscillator for ultrasonic extraction for about 30 min, centrifuge at low speed, transfer the supernatant, add 40 mL of 80% acetonitrile aqueous solution of 2% ammonia to the residue, repeat the above operation once, and combine the supernatant; the supernatant is fully automatic The solid-phase extraction instrument was used for program elution and purification, using WatersOasis MAX 6cc (500mg) anion exchange column, the enrichment and elution program time is shown in Table 1, to achieve the purification and enrichment of 80 mL extraction solution;

[0042] Table 1. Fully automatic solid-phase ext...

Embodiment 11-20

[0045] Embodiment 11-20: Determination of the content of rice yeast acid in dry corn

[0046] 2) After crushing 10 batches of dried white fungus purchased in the market, weigh 20 g and place them in a conical flask, add 40 mL of 2 % ammonia water and 80 % acetonitrile aqueous solution as the extraction solvent, mix well, and soak for 1 h at room temperature in the dark. Place in an ultrasonic oscillator for ultrasonic extraction for about 30 min, centrifuge at low speed, transfer the supernatant, add 40 mL of 80% acetonitrile aqueous solution of 2% ammonia to the residue, repeat the above operation once, and combine the supernatant; the supernatant is fully automatic The solid-phase extraction instrument was used for program elution and purification, using WatersOasis MAX 6cc (500mg) anion exchange column, the enrichment and elution program time is shown in Table 1, to achieve the purification and enrichment of 80 mL extraction solution;

[0047] Table 1. Fully automatic solid...

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Abstract

The invention discloses a method for rapidly measuring a content of bongkrekic acid in food by automatic solid phase extraction-ultra performance liquid chromatography. The method comprises steps of pretreatment of food samples, purification of extracted solution and HPLC analysis to obtain the content of bongkrekic acid in the food samples; and results are proved. The method provided by the invention replaces a traditional manual column passing method with an automatic solid phase extraction instrument to realize automation, reduce labor costs and personal errors, realize controllability of solid phase extraction velocity, improve repeatability and accuracy of experiments and shorten a sample treatment cycle; the method optimizes extraction conditions, chromatographic conditions and the like to obtain an excellent separation degree and chromatographic peak, has advantages of high sensitivity, high recovery rate and relatively short pretreatment cycle, meets requirements on detection of the content of bongkrekic acid in food, provides a reference for a laboratory to carry out relevant detections and plays an active role in ensuring food safety.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and in particular relates to a method for quickly determining the content of rice fermented acid in food by mixed anion automatic solid-phase extraction-ultra-high performance liquid chromatography. Background technique [0002] Bongkrekic acid (BKA) is a fat-soluble acidic compound with the molecular formula C 28 h 38 o 7 , with a relative molecular mass of 486.6, is one of the metabolites of Pseudomonas cocos subspecies fermented rice noodles. It exists in fermented food, spoiled white fungus and other foods. It is highly toxic and will cause nausea, vomiting, and convulsions , shock and other poisoning symptoms, damage the liver, brain nerve cells and kidney tissue, the fatality rate is as high as 40% to 100%, causing many food poisoning incidents in our country, and strict precautions are required. Oryzanic acid has an effect on the mitochondrial permeability transition pore....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 周霞罗金文陈万勤刘柱梁晶晶丁宇琦徐潇颖赵超群傅红雪
Owner ZHEJIANG INST FOR FOOD & DRUG CONTROL
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