Graphitized carbon SPE column-based rapid detection method for patulin in apple juice

A technology of graphitized carbon and patulin, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems not mentioned about graphitized carbon, etc., and achieve the effect of strong practical application value, simple production method and simple operation steps

Pending Publication Date: 2021-07-30
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention does not mention that graphitized carbon is capable of adsorbing other mycotoxins than aflatoxins M1 and M2

Method used

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  • Graphitized carbon SPE column-based rapid detection method for patulin in apple juice
  • Graphitized carbon SPE column-based rapid detection method for patulin in apple juice
  • Graphitized carbon SPE column-based rapid detection method for patulin in apple juice

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: graphitized carbon SPE column

[0041] 1. Filler screening

[0042]For 16 common Cleanert adsorbents (C18, Alumina-B, Alumina-N, Florisil, PSA, PestiCarb, NH2, Silica, Alumina-A, COOH, CN, Diol, PRS, SAX, SCX, PS), weigh each 150mg was poured into the empty tubes of SPE column with the lower sieve at the bottom, and the upper sieve was placed above the adsorbent, and pressed tightly to prepare 16 kinds of SPE columns.

[0043] The filler was screened based on the adsorption rate of patulin. Take 2 mL of patulin standard solution (50 μg / L) to load the sample, pass through the column in a straight-through manner, collect the effluent from all the above 16 SPE columns, pass through a 0.22 μm filter membrane, and perform HPLC-PDA detection. figure 1 It is a histogram of the adsorption rate of patulin on 16 self-made SPE columns. Depend on figure 1 It can be seen that PestiCarb has the best adsorption effect on patulin, and no patulin was detected in the ef...

Embodiment 2

[0054] Embodiment 2: purification parameter design

[0055] 1. Organic solvent selection

[0056] Accurately draw 2mL of the spiked apple juice (PAT spiked concentration is 50 μg / kg), gravity acts on the graphitized carbon SPE column prepared in Example 1, and blows dry. Add 4mL of different elution solvents, elute by gravity, blow dry, and completely collect the eluate in a 10mL plastic centrifuge tube. Add 20 μL of acetic acid to the eluate, and blow it with nitrogen at 40°C until nearly dry. Accurately add 1.0 mL of 1% acetic acid aqueous solution to redissolve, vortex for 30 s, and pass through a 0.22 μm filter membrane for HPLC-PDA detection.

[0057] figure 2 It is a histogram of the recovery rate of patulin eluted by different organic solvents. Depend on figure 2 It can be seen that the recovery rate of ethyl acetate is the highest, and the recovery rate of dichloromethane is the lowest, but both are above 80%, which can meet the detection requirements of HPLC. ...

Embodiment 3

[0069] Accurately draw 4mL of apple juice, pass through the graphitized carbon SPE column prepared in Example 1 by gravity, and blow dry. Add 6 mL of dichloromethane, elute by gravity, blow dry, and completely collect the eluate in a 10 mL plastic centrifuge tube. Add 20 μL of acetic acid to the eluate, and blow it with nitrogen at 40°C until nearly dry. Accurately add 1.0 mL of 1% acetic acid aqueous solution, vortex for 30 s, and pass through a 0.22 μm aqueous phase filter membrane for HPLC-PDA detection.

[0070] The detection conditions are as follows:

[0071] Instrument model: Waters 2695 with PDA detector (diode array detector);

[0072] Chromatographic column: Agilent TC C18 column (250mm×4.6mm, 5μm);

[0073] Column temperature: 40°C;

[0074] Mobile phase: A phase is water, B phase is acetonitrile, gradient elution, the elution program is shown in Table 1;

[0075] Injection volume: 50μL;

[0076] Detection wavelength: 276nm;

[0077] Flow rate: 1.0 mL / min.

...

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Abstract

The invention belongs to the field of quality safety detection of fruits, vegetables and products thereof, and particularly discloses a graphitized carbon SPE column-based rapid detection method for patulin in apple juice, which comprises the following specific steps of (1) preparing a graphitized carbon SPE column for purifying patulin by taking graphitized carbon as a filler, (2) enabling the apple juice to be detected to directly pass through the column, and eluting the patulin adsorbed by the apple juice with an organic solvent to obtain a purified solution, and (3) carrying out nitrogen blowing, redissolving and membrane passing on the purified liquid, and then detecting the content of patulin in the apple juice by using HPLC-PDA. The purification column is designed by utilizing the adsorption effect of the graphitized carbon filler on the patulin, the purification column is used only by two steps of sample loading and elution, the steps of sample pretreatment, column activation and leaching are omitted, the purification effect is good, the sample pretreatment efficiency is improved, and the detection cost is reduced.

Description

technical field [0001] The invention belongs to the field of quality and safety detection of fruits and vegetables and their products, in particular to a rapid detection method for patulin in apple juice based on a graphitized carbon SPE column. Background technique [0002] Patulin (PAT), also known as patulin, patulin, and coral penicillin, is a secondary metabolite produced by various fungi such as Penicillium and Aspergillus, and is commonly found in various molds. Among the changed fruits, it is stable under acidic conditions, but easy to decompose under alkaline conditions, and has the highest pollution rate among apples and their products. In 2016, a batch of imported apple juice with patulin exceeding the standard was detected at Ningbo port. In 2020, Pick’d Cloudy Apple Juice was urgently recalled by the Australian Food Standards Agency due to the detection of excessive patulin. Ingestion of patulin-contaminated food can cause gastrointestinal discomfort, nausea a...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/52G01N30/60G01N30/74
CPCG01N30/02G01N30/06G01N30/36G01N30/34G01N30/52G01N30/60G01N30/74G01N2030/524Y02A50/30
Inventor 张巧艳王夏君王栩鸣胡桂仙郭辉
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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