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Method for detecting tobacco specific nitrosamine by liquid phase chromatography and series mass spectrometry

A technology of tandem mass spectrometry and liquid chromatography, applied in the field of detection of N-nitrosamines, can solve the problems of poor purification effect and low recovery rate, achieve improved purification effect and recovery rate, easy operation, and strong instrument versatility Effect

Active Publication Date: 2006-12-06
CHINA TOBACCO HUNAN INDAL CORP
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Problems solved by technology

[0003] The invention aims to solve the problems of poor purification effect and low recovery rate in the detection of tobacco-specific N-nitrosamines, and provides a method for detecting tobacco-specific nitrosamines that can improve the purification effect and recovery rate, is easy to operate, and has strong instrument versatility. Amine method

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] First add 1.0ml 300ng / ml trimethyl to the 92mm diameter Cambridge filter disc that captured the smoke of 20 9mg 555 brand cigarettes 13 C 3 Mark the caffeine methanol solution, then add 30ml each of pH 4.3 citric acid-phosphate buffer solution containing 53mmol / l citric acid and 20mmol / l ascorbic acid and 30ml of cyclohexane, and shake the filter for co-extraction. After separating the organic phase extract, N 2 Concentrate to about 1ml under protection, then add 1ml of 0.1mol / l hydrochloric acid to it for acidification, after phase separation, add 1mol / l sodium hydroxide solution dropwise to the water phase to pH 7.0. The obtained aqueous phase solution was quantitatively transferred to an Oasis HLB solid-phase extraction column from Waters, USA, which had been equilibrated successively with 3 ml of methanol and 3 ml of distilled water, then rinsed with 3 ml of 5% aqueous methanol, and eluted with 5 ml of methanol. The eluate was concentrated to 1 ml for LC / MS / MS ana...

Embodiment 2

[0018] Using methanol as a solvent, configure a series of mixed standard sample solutions according to the concentration range in Table 1, wherein trimethyl 13 C 3 Labeled caffeine is 300ng / ml; then carry out LC / MS / MS analysis and detection under the above-mentioned experimental conditions, with component peaks on the chromatogram and trimethyl 13 C 3 The area ratio of the marked caffeine peak is the response signal. According to the three parallel measurement results of the six mixed standard solutions, the standard curves of the four components of NNN, NNK, NAT and NAB were established, and the linear correlation coefficients of each standard curve were in order It is 0.9992, 0.9980, 0.9990 and 0.9992, showing that the response signal is significantly linearly correlated with the component concentration; 3 times of the standard deviation of the results of 5 parallel measurements of the lowest concentration mixed standard sample solution determines the method detection limit...

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PUM

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Abstract

The present invention relates to liquid phase chromatography-tandem mass spectrometry process for detecting specific tobacco fume nitrosamine content. The detection process includes: trapping tobacco fume with filtering sheet, adding internal standard substances, vibration extracting the filtering sheet with citric acid-phosphate buffering solution and cyclohexane, concentrating the organic phase extracted liquid in N2 protection, acidifying with hydrochloric acid, phase separating, neutralizing water phase with alkali solution, transferring the water phase solution into reverse chemical bonded solid phase extracting column, leaching with polar organic solvent aqua, eluting with polar organic solvent aqua, concentrating elutent, and analyzing in LC / MS / MS instrument quantitatively based on the area ratio between the component peak and the internal standard substance peak. The present invention has high repeatability, high recovering rate and low detection limit.

Description

technical field [0001] The invention relates to a method for detecting N-nitrosamines, in particular to a method for detecting tobacco-specific N-nitrosamines. Background technique [0002] Tobacco-specific N-nitrosamines are a class of compounds that only exist in tobacco and its products. Although they are generally stable under physiological conditions, they are strongly carcinogenic through metabolic activation in vivo. In order to reduce the possible harm of tobacco-specific N-nitrosamines to the health of smokers and passive smokers, control and reduce their content in tobacco and its products has become an important issue. Tobacco-specific N-nitrosamines Content will become an important indicator to measure the quality of tobacco products. Therefore, since the 1990s, domestic and foreign studies have been carried out on the detection methods of tobacco-specific nitrosamines in tobacco. However, because the composition of tobacco and cigarette ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/88
Inventor 毛友安钟科军魏万之戴云辉魏新亮卢红兵李艳春
Owner CHINA TOBACCO HUNAN INDAL CORP
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