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A comprehensive detection method for volatile n-nitrosamine compounds in food

A technology of nitrosamines and detection methods, which is applied to measurement devices, instruments, material analysis by electromagnetic means, etc. nitrosamine compound distinction and other issues, to achieve the effect of good promotion and use value, easy real-time tracking, and saving test costs

Inactive Publication Date: 2016-04-06
HUNAN UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The existing national standards only target a limited number of 4 kinds of nitrosamine compounds, and nearly 300 kinds of nitrosamine compounds have been found, and the limited 4 kinds obviously cannot represent the toxicity of all nitrosamine compounds;
[0005] (2) The existing method utilizes gas phase (or liquid phase) chromatography-mass spectrometry, which has powerful functions in the analysis of organic matter, but does not consider the structural characteristics of nitrosamines themselves, and cannot effectively separate the nitrosamines. Nitramine compounds can be effectively distinguished from other organic substances;
[0006] (3) For N-nitroso compounds separated and extracted from food or other biological materials, the existing methods are prone to false positive results due to the interference of accompanying impurities
[0007] (4) Existing methods do not make full use of the value of differences in different ion sources when detecting nitrosamine compounds, such as the effects of EI and ESI ion sources on samples are very different;
[0008] (5) The detection of nitroso compounds by spectrophotometry has serious interference, and the selectivity of photometry is poor
[0009] At present, the full detection of nitrosamine compounds in food is mainly based on chemical methods, and most of them are still in the theoretical research stage. There is no fast and accurate full detection method

Method used

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  • A comprehensive detection method for volatile n-nitrosamine compounds in food
  • A comprehensive detection method for volatile n-nitrosamine compounds in food
  • A comprehensive detection method for volatile n-nitrosamine compounds in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Sample distillation and extraction: Weigh 50 g of crushed commercially available bacon products, use a simultaneous extraction and distillation device to carry out two steps of distillation and extraction at the same time, put the weighed sample in a sample bottle, add ultrapure water 100mL and internal standard two Connect 40ml of methyl chloride to the simultaneous extraction and distillation device, start heating for distillation and ultrasonic extraction, and collect condensate. The distillation temperature is controlled at 110°C, and the collection temperature is controlled at 45°C. When the distillate begins to drip from the phase separation tube Distillation ends after 40-60 minutes;

[0052] Concentration and constant volume: Concentrate the extract in the collection bottle to a volume of <1.0mL, dry it with anhydrous sodium sulfate, transfer the concentrated solution into a 2.0mL brown sampling bottle, wash the collection bottle with methanol, and mix the washin...

Embodiment 2

[0062] Adopt the same method as Example 1, the difference is: the food to be tested is traditional kimchi.

[0063] After calculation, the total content of nitrosamine compounds in the traditional kimchi used in this example is 4.84ng / g, as shown in Table 2.

[0064] Table 2 The content and total amount of each nitrosamine compound in pickles in Example 2 of the present invention

[0065]

[0066] The analytical result figure of embodiment 2 traditional kimchi is as follows image 3 shown, from image 3 It can be seen that there are 100-105 kinds of volatile organic components detected in traditional kimchi in Example 2, but it can be seen from the enlarged picture of the probe signal that only 27 kinds contain probe signals 30 and 44. The gas chromatograms of the 27 nitroso compounds corresponding to the mass spectra are as follows Figure 4 shown.

Embodiment 3

[0068] Adopt the same method as Example 1, the difference is: the food to be tested is edible betel nut.

[0069] After calculation, the total content of nitrosamine compounds in the edible betel nut used in this example is 115.3 ng / g, as shown in Table 3.

[0070] Table 3 The content and total amount of each nitrosamine compound in the embodiment of the present invention 3 betel nuts

[0071]

[0072] Example 3 The analytical result figure of edible betel nut Figure 5 shown, from Figure 5 It can be seen that there are 70-75 kinds of volatile organic components detected in the edible betel nut in Example 3, but from the enlarged picture of the probe signal, it can be seen that there are only 14 kinds of volatile organic components containing probe signals 30 and 44. The gas chromatograms of the 14 nitroso compounds corresponding to the mass spectra are as follows Figure 6 shown.

[0073] It is worth noting that the present invention has analyzed 4 parts of bacon prod...

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Abstract

The invention discloses a comprehensive detection method for volatile N-nitrosamine compounds in food. Including sample extraction, qualitative analysis, quantitative determination, result analysis and result conversion, sample extraction includes distillation, extraction, concentration and constant volume; gas chromatography-mass spectrometry is used for qualitative analysis; gas chromatography is used for quantitative determination. The present invention adopts NO and N2O dual-probe ion technology to fully detect N-nitrosamine compounds in food, which can not only accurately screen out the types of N-nitrosamine compounds, but also effectively exclude non-N-nitrosamine compounds. Compounds, avoiding false detection and missed detection; can distinguish nitrosamine compounds from numerous volatile organic components at one time, and can directly qualitative and quantitative limited, a small number of related nitrosamine compounds, greatly saving Analysis time.

Description

technical field [0001] The invention relates to the field of food safety, in particular to a comprehensive detection method for volatile N-nitrosamine compounds in food. Background technique [0002] N-nitrosamine compounds belong to nitroso compounds, are highly toxic organic compounds, have carcinogenic, teratogenic and mutagenic effects, and are one of the four major food pollutants today. In fresh food, the content of nitrosamine compounds is very low, but in the process of transportation, processing, storage, etc., it is easy to produce various N-nitrosamines due to factors such as lack of oxygen, heat accumulation, microorganisms, and mildew. Amine compounds: According to data, different sources of food, different types of microorganisms, and different storage times will produce different types of N-nitrosamine compounds. Recently, scientists have used an inorganic reducing agent (such as: cuprous chloride; CuCl) to denitrosamine the chemiluminescence method to detect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N27/62
Inventor 周再春成奋民马金辉袁晟
Owner HUNAN UNIV OF SCI & TECH
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