Method for simultaneously and quantitatively detecting content of ethyl carbamate and phthalate in distilled white wine

A technology of urethane and phthalates in the medium, which is applied in the field of simultaneous quantitative detection of urethane and phthalates in distilled liquor, and can solve the problems of cumbersome operation and long time of detection methods , to achieve the effect of easy promotion, simple operation and short analysis time

Active Publication Date: 2013-10-09
SICHUAN JIANNANCHUN GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved by the present invention is that

Method used

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  • Method for simultaneously and quantitatively detecting content of ethyl carbamate and phthalate in distilled white wine
  • Method for simultaneously and quantitatively detecting content of ethyl carbamate and phthalate in distilled white wine
  • Method for simultaneously and quantitatively detecting content of ethyl carbamate and phthalate in distilled white wine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Wash the 50mL volumetric flask with the wine sample to be tested for 2-3 times. After cleaning, add about 10mL of the wine sample to be tested into the volumetric flask, and then add 30μL of internal standard Ⅰ and 30μL of internal standard Ⅱ to the volume with a pipette gun. Finally, use the wine sample to be tested to make up the volume to the mark, shake gently, and mix well. Pour the mixed wine sample to be tested with the internal standard into the Agilent sample bottle for gas chromatography-mass spectrometry analysis and detection.

[0074] The conditions of gas chromatography are: use ZB-WAXplus capillary chromatographic column for separation, the length of chromatographic column is 30m, the inner diameter is 0.25mm, the film thickness is 0.25μm; Sample, column flow rate 1mL / min; temperature rise program: keep at 40°C for 2min, rise to 160°C at 10°C / min, then rise to 230°C at 30°C / min, and hold for 15.6min.

[0075] The conditions of mass spectrometry are: elec...

Embodiment 2

[0099] Embodiment 2 Precision and sensitivity of the inventive method

[0100] According to the method of Example 1, a wine sample was measured in parallel 5 times, and the precision results of the sample were as shown in Table 1:

[0101] Table 1 Precision of the inventive method

[0102]

[0103] The results in Table 1 show that the RSD (relative standard deviation) is less than 10%, indicating that the content of urethane and phthalates in wine samples can be accurately determined.

[0104] Quantitation limit and detection limit reflect the sensitivity of the detection method, and only when it is significantly lower than the maximum residue limit can it be used for determination. The content when the signal-to-noise ratio S / N=3 is the detection limit; the content when the signal-to-noise ratio S / N=10 is the quantification limit. The results in Table 2 show that the sensitivity of this method is high.

[0105] Table 2 Sensitivity of the inventive method

[01...

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Abstract

The invention belongs to the field of white wine detection, particularly relates to a method for simultaneously and quantitatively detecting the content of ethyl carbamate and phthalate in the distilled white wine and aims to solve the problems the existing method for detecting is complex in operation and consumes long time. The method comprises the following steps of: (a) adding an internal standard substance I and an internal standard substance II into a white-wine sample, and (b) detecting by adopting a gas chromatograph mass spectrometer, monitoring and quantitating by using selected irons, and obtaining the content of the ethyl carbamate and the phthalate in the distilled white wine by adopting the internal standard method. The method provided by the invention has good reproducibility, is accurate and is low in detection cost, thereby being easy to popularize.

Description

technical field [0001] The invention belongs to the field of liquor detection, in particular to a method for simultaneously quantitatively detecting the contents of ethyl carbamate and phthalate in distilled liquor. technical background [0002] Ethyl carbamate (EC for short), also known as urethane, is a naturally formed by-product of fermented food during fermentation and storage. After research, ethyl carbamate in distilled liquor is produced by the spontaneous reaction of carbamyl compounds and ethanol. In 1987, the International Cancer Research Center (IARC) listed EC as a group2B: possible carcinogen; in 2004, the NTP program included EC in the list of "substances that are reasonably expected to cause cancer"; in 2007, IARC re-evaluated EC, and lead , mercury and acrylamide are listed in group2A. At present, Chinese patent 201210441000.6 discloses "High Performance Liquid Chromatography-Mass Spectrometry Detection Method for Ethyl Carbamate in Distilled Liquor". ), ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 陈勇李开雁李冰川
Owner SICHUAN JIANNANCHUN GRP CO LTD
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