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LC-MS/MS positive ion mode detection method of EDTA in wine

A technology of LC-MS and detection methods, which is applied in the direction of measuring devices, material separation, instruments, etc., can solve problems such as unsatisfactory, time-consuming, high energy consumption, etc., and achieve the effects of avoiding influence, high accuracy, and avoiding method errors

Inactive Publication Date: 2015-12-30
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used detection methods include high performance liquid chromatography, gas chromatography, ion chromatography and capillary electrophoresis, etc., but there are problems of complicated operation, long time consumption, high energy consumption and low detection sensitivity, especially Low problem, unable to meet the detection of most foods containing trace amounts of EDTA

Method used

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  • LC-MS/MS positive ion mode detection method of EDTA in wine
  • LC-MS/MS positive ion mode detection method of EDTA in wine
  • LC-MS/MS positive ion mode detection method of EDTA in wine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0095] The LC-MS / MS assay method of EDTA in the embodiment 1 test sample

[0096] 1. Pretreatment of samples to be tested

[0097] (1) Take 1.00mL of the beer sample to be tested with a 1000μL pipette gun, put it in a heat-resistant test tube with a seal, add 1.00mL of 20.0mg / L phenylboronic acid solution and 8.00mL of 10% isobutylamine methanol solution, and place in Oscillate at room temperature and constant temperature for 20.0 minutes in a water bath shaker;

[0098] (2) Use a 1.0mL syringe to pass through a 0.2μm microporous membrane;

[0099] (3) Take 0.20mL of the above solution to the injection bottle, then add 0.80mL of 10% isobutylamine methanol solution, shake well, and measure by liquid chromatography tandem mass spectrometry.

[0100] What needs to be emphasized here is that when phenylboronic acid is added for derivatization reaction, the shaker must be shaken for a long enough time to ensure that the sugars in beer react fully with phenylboronic acid, minimi...

Embodiment 2

[0163] The mensuration of EDTA in the different wine samples of embodiment 2

[0164] 1. (1) After using the method for pretreatment of the sample to be tested described in Example 1 to pretreat various alcohol samples, then perform liquid chromatography tandem mass spectrometry according to the instrument parameters and measurement conditions described in Example 1, and finally Calculate the EDTA content in the wine sample to be tested.

[0165] All wine samples used were commercially available.

[0166] (2) According to the existing international standards for the identification of the quality of wine samples, GB2760-2011 stipulates that the residual amount of EDTA in beverages shall not exceed 30mg / kg. If the calculation result of the mass concentration of EDTA-2Na in the measured sample exceeds 30mg / kg, it can be identified. for substandard products.

[0167] 2. The test results are shown in Table 5. Dozens of imported and domestic beer and wine samples were tested, an...

Embodiment 3

[0171] Example 3 Influence of primary amines on measurement results—positive ion mode realizes accurate detection of EDTA

[0172] 1. In the pretreatment of samples by the detection method of the present invention, primary amines are used to dechelate EDTA-transition metals, so as to avoid the interference of metal ions in the solution on the EDTA content.

[0173] In LC / MS-MS, under the two ionization modes of positive ion and negative ion, no EDTA-metal chelate was detected in the Q1 scan, indicating that the EDTA-transition metal was dechelated, and it was proved by experiments that amines The dechelation ability of the compound, the result is primary amine > secondary amine > tertiary amine, as attached image 3 shown.

[0174] Secondly, when using different concentrations of Fe(III) and Cu(II) for interference experiments, the recovery rate of EDTA in the sample is between 88% and 105%, as shown in the attached Figure 4 As shown, it shows that these two metal ions wi...

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Abstract

The invention discloses an LC-MS / MS positive ion mode detection method of EDTA in food (particularly wine). The method comprises the steps that 1, a sample to be detected is pretreated, wherein 11, the sample to be detected is sucked into a container capable of being closed, a 20.0 mg / L boric acid solution and a 10% amine methanol solution (preferentially, a 10% butyl amine methanol solution) are added, and the container is closed for even mixing; 12, the solution obtained through the step 11 passes through a microporous filtering film with the pore diameter being 0.1-0.5 micrometer to obtain a filtrate; 2, the filtrate is placed into a sample bottle, then, an amine methanol solution is added, sufficient and even shaking is carried out, and then detection is carried out through liquid chromatogram and tandem mass spectrum. The method can qualitatively and quantitatively analyze and detect EDTA in food such as wine, and is good in stability, accurate and sensitive, the qualitative limit is 0.0001 mg / kg, and the quantitative limit is 0.001 mg / kg; the detection method is simple, method errors are avoided, consumed time is short, energy consumption is low, and the application and popularization prospect is good.

Description

technical field [0001] The invention belongs to the technical field of food detection. More specifically, it relates to a LC-MS / MS positive ion mode detection method for EDTA in wine. Background technique [0002] Ethylenediaminetetraacetic acid (EDTA) is a white crystalline granule or powder, insoluble in water, easy to form stable water-soluble complexes with multivalent ions of iron, copper, calcium and other metals at room temperature to prevent Discoloration, deterioration, and oxidation and loss of vitamin C and other nutrients caused by trace amounts of metal multivalent ions. In recent years, EDTA has been added to wine and other foods as a new type of antioxidant to protect nutrients and increase stability. [0003] However, EDTA has many negative effects on the human body, such as irritating the skin and mucous membranes, causing asthma, skin rashes, etc. It is a substance that may cause allergies. After being ingested, it will cause calcium deficiency, lower blo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 韦晓群李志勇谢力庄林洲刘青王志元陈文锐席静
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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