Method of determining specific aromatic amine released by azodye in cigarette paper through bonded phase chromatography-tandem mass spectrometry

A technology of tandem mass spectrometry and convergence chromatography, which is applied in the field of determination of carcinogenic aromatic amines, can solve the problems that liquid chromatography cannot be separated well, qualitative ability is not as good as tandem mass spectrometry, and sensitivity and qualitative ability are poor, so as to achieve fast and simple sensitivity, Avoid matrix effect, high recovery effect

Inactive Publication Date: 2017-07-14
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Problems solved by technology

However, these methods have certain limitations. GC and HPLC usually have poor sensitivity and qualitative capabilities, so false positive results may occur
GC-MS and HPLC-MS have high sensitivity and certain selectivity, but they are also susceptible to matrix interference in complex matrix systems, and their qualitative capabilities are not as good as tandem mass spectrometry
Chinese patent (201410041729.3) discloses "A Determination Method for Prohibited Azo Dyes in Cigarette Paper", which involves the detection of aromatic amines. This patent combines liquid-liquid extraction and liquid chromatography tandem mass spectrometry technology, which greatly improves the analytical sensitivity and The detection efficiency is high, but because these aromatic amines have similar structures and most of them have isomers, ordinary liquid chromatography cannot separate these aromatic amines very well, and occasionally there will be false positive results For example, 2,4-dimethylaniline and 2,6-dimethylaniline are isomers, which cannot be separated well by ordinary liquid chromatography

Method used

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  • Method of determining specific aromatic amine released by azodye in cigarette paper through bonded phase chromatography-tandem mass spectrometry
  • Method of determining specific aromatic amine released by azodye in cigarette paper through bonded phase chromatography-tandem mass spectrometry
  • Method of determining specific aromatic amine released by azodye in cigarette paper through bonded phase chromatography-tandem mass spectrometry

Examples

Experimental program
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Effect test

example 1

[0036] 1. Instruments and reagents:

[0037] Tert-butyl methyl ether and methanol are chromatographic grade reagents, sodium hydroxide and sodium sulfate are analytical reagents; distilled water meets the requirements of first-grade water in GB / T 6682.

[0038] UPCs 2 -MS / MS quadrupole tandem mass spectrometer; water bath constant temperature oscillator; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0039] 2. Sample handling:

[0040] Weigh 1.0 g sample (accurate to 0.0001 g); put the fragments in a 50 mL Erlenmeyer flask with a stopper, place the sample in a 50 mL stoppered centrifuge tube, add 15 mL of citric acid buffer preheated to 70±2°C Shake vigorously to soak the sample, and place it in a 70±2°C water bath for 30 minutes; add 3 mL of 200 mg / mL sodium dithionite aqueous solution, keep it at 70±2°C, react for 30 minutes, and then place the centrifuge tube in an ice-water bath Cool to room temperature within 2 minutes;

[0041] Add 0.5 mL of 40% ...

example 2

[0045] According to the determination method described in Example 1, another cigarette paper sample was selected, and the p-chloroaniline content in the sample was 2.25 mg / kg.

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Abstract

The invention relates to a method of determining specific aromatic amine released by azodye in cigarette paper through bonded phase chromatography-tandem mass spectrometry, belonging to the technical field of physical and chemical inspection of residual harmful substances in paper. According to the method, the azodye is reduced to aromatic amine by using sodium hydrosulfite in a weak acidic buffer solution, then the aromatic amine is subjected to solid-phase, purification and nitrogen-blow concentration, afterwards a bonded phase chromatography-tandem mass spectrometry combination instrument is used for determination, and an internal standard method is used for fixing quantity. The method has the beneficial effects that the shortcomings of a sample treatment method in the prior art are overcome; a sample pretreatment method and instrument detection conditions are optimized according to paper samples; the disturbance of matters with similar structures to target objects can be reduced; and the method has the advantages of accurate operation, high recovery rate, short separation time, fastness, simplicity, convenience, high sensitivity and the like.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical inspection of harmful substance residues in tobacco materials, and mainly relates to the determination technology of carcinogenic aromatic amines released by azo dyes. Specifically, azo dyes are reduced to aromatic amines by sodium dithionite in a citric acid buffer solution , and then purified by solid phase extraction, concentrated by nitrogen blowing, determined by convergence chromatography tandem mass spectrometry, and quantified by internal standard method. Background technique [0002] Azo dyes refer to dyes that contain an azo group -N=N- in their molecular structure. It is generally believed that the structure of azo dyes itself will not have harmful effects on the human body, but there are some azo dyes synthesized with "arylamine intermediates", because after long-term contact with human skin, the skin on the surface of the human body will be affected. In the weak acid en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045G01N2030/062
Inventor 杨飞邓惠敏严俊周芸唐纲岭李小兰李中皓王颖孟冬玲陆冰琳
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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