Method for detecting content of N-nitrosodimethylamine in beer

A technology of dimethylnitrosamine and beer, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high specificity requirements of instruments, difficulty in popularization and application, and large solvent consumption, so as to achieve less actual consumption , Convenient promotion and application, good selectivity and accuracy

Inactive Publication Date: 2015-04-29
ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the detection of N-dimethylnitrosamine in beer, the national standard GB / T5009.26-2003 pretreatment adopts conventional liquid-liquid extraction method and distillation method. As a traditional pretreatment technology, this method can be well completed The separation of target components usually requires multiple extractions and long-term distillation to ensure the recovery rate, and further transfer and concentration are required. The operation is cumbersome, the pretreatment is time-consuming and laborious, and the solvent consumption is large.
GB / T5009.26—2003 stipulates that the instrument detection methods include gas chromatography thermal energy detector method and high resolution gas chromatography method. The latest national food safety standard "Determination of N-nitrosamine compounds in food" draft for comments adopts three methods : The first method is gas chromatography-nitrogen chemical reflective detector method, the second method is gas chromatography-thermal energy analyzer method, and the third method is gas chromatography high-resolution mass spectrometry. The biggest disadvantage of these methods is the high specificity requirements for instruments , there are very few testing institutions in China that have the above-mentioned instruments, it is difficult to popularize and apply, and the cost of the instruments is high. For example, the price of a high-resolution mass spectrometer is several million, and the procurement cost is too high
Therefore, the standard is useless and difficult to be accepted

Method used

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  • Method for detecting content of N-nitrosodimethylamine in beer
  • Method for detecting content of N-nitrosodimethylamine in beer
  • Method for detecting content of N-nitrosodimethylamine in beer

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Beer extraction: take 100mL beer, ultrasonically degas it in an ultrasonic cleaner for 5 minutes, then measure 10mL into a 50mL centrifuge tube, add 100μL 2.0mg / L internal standard D6-N, N-dimethylnitrosamine standard Application solution, that is, 200ng internal standard D6-N, N-dimethylnitrite, mix well, add 3.0g sodium chloride to dissolve to saturation, add 15mL dichloromethane, vortex extract for 2min, then centrifuge at 10000rpm for 4min, discard The upper aqueous phase and the dichloromethane layer were dehydrated with anhydrous sodium sulfate, and then blow-dried with nitrogen at room temperature to less than 0.1 mL (not dry), then added 1 mL of cyclohexane, and ultrasonically mixed to obtain a solution to be purified.

[0035] (2) Purification of beer: Take a SILICA / PSA glass column (1000mg / 6mL), first wash the activation column with 3mL dichloromethane and 5mL cyclohexane in sequence, then pass all the solution through the column, first use 5mL dichlorometh...

Embodiment 2

[0042] Take beer blank sample 10mL, add 100μL 2.0mg / L N-dimethylnitrosamine use solution, obtain beer standard sample solution A, the concentration of N-dimethylnitrosamine in beer standard sample solution A is 20μg / L.

[0043] Take beer blank sample 10mL, add 25 μ L 2.0mg / L N-dimethylnitrosamine use solution, obtain beer standard sample solution B, the concentration of N-dimethylnitrosamine in beer standard sample solution B is 5 μg / L.

[0044] Take beer standard sample solution A and beer standard sample solution B respectively, and operate according to steps (1) to (2) of Example 1:

[0045] (1) Measure 10mL to 50mL centrifuge tube, add 100μL 2.0mg / L internal standard D6-N, N-dimethylnitrosamine standard application solution, that is, 200ng internal standard D6-N, N-dimethylnitrosamine , mix well, add 3.0g sodium chloride to dissolve to saturation, add 15mL dichloromethane, vortex extract for 2min, then centrifuge at 10000rpm for 4min, discard the upper aqueous phase, deh...

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Abstract

The invention discloses a method for detecting N-nitrosodimethylamine in beer. The method comprises the followings steps: adding a D6-N-nitrosodimethylamine internal standard substance into a beer sample, adding sodium chloride to dissolve to saturation, extracting by using dichloromethane, concentrating extracting liquid, dissolving by cyclohexane, purifying dissolved liquid by an SILICA/PSA solid phase extraction column, eluting and collecting by dichloromethane, taking 1.01 [mu]l of a sample for feeding, and analyzing and detecting by a gas chromatograph-mass spectrometer, establishing a standard curve by using an internal standard method, detecting and calculating so as to obtain the content of N-nitrosodimethylamine in the beer. According to the method, after extraction by dichloromethane, the SILICA/PSA solid phase extraction column is adopted for purification, so that interfering substances are effectively removed, and interfering substance removal capacity is high. The gas chromatography-low-resolution mass-spectrometry is adopted for determining, so that requirements for the instrument are low, the cost is low, and the method is easy to popularize and use. According to the embodiment of the invention, under the condition that interfering ions 44 and 73 are added, a target object can be measured accurately, so that the fact that the method is high in reliability is indicated.

Description

(1) Technical field [0001] The invention relates to a method for detecting the content of N-dimethylnitrosamine in beer. (2) Background technology [0002] Wine, meat and fish pickled products, soybean products and other foods contain N-dimethylamine nitroso, N-diethylamine nitroso and so on. Nitrosamine compounds have certain acute toxicity and strong carcinogenicity, and mainly cause hepatic necrosis and hemorrhage. People pay more attention to their carcinogenicity. So far, there are more than 300 kinds of nitrosamines, among which N-dimethyl sulfide Nitramine is one of the most representative substances. The sources of nitrosamines in food are as follows: (1) the effect of nitrite in salt during pickling, such as salted fish, bacon, etc.; (2) nitrogen in the air is oxidized into nitrogen oxides during heating and drying Function, such as beer, milk powder, soy products. In recent years, the detection of volatile nitrosamines has shown that the N-dimethylamine nitrosam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 吴平谷沈向红王立媛胡争艳
Owner ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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