Method for detecting NNAL (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol) and NNA in cut tobacco and cigarette smoke

A cigarette smoke and shredded tobacco technology, applied in the field of tobacco chemical inspection, can solve the problems of difficult detection, low nitrosamine content, complex tobacco extract and smoke matrix, and achieve easy popularization and application, low detection limit, and stability Good results

Active Publication Date: 2015-07-15
HONGYUN HONGHE TOBACCO (GRP) CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, due to the low content of tobacco-specific nitrosamines in shredded tobacco and cigarette smoke, and the complexity of tobacco extracts and smoke matrices, it is very difficult to detect NNAL and NNA in shredded tobacco and cigarette smoke. The industry is unable or has not carried out the detection of NNAL and NNA in cigarette shredded tobacco and cigarette smoke

Method used

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  • Method for detecting NNAL (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol) and NNA in cut tobacco and cigarette smoke
  • Method for detecting NNAL (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol) and NNA in cut tobacco and cigarette smoke

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The mensuration of embodiment 1 cigarette sample NNAL and NNA release

[0026] Chemical reagent preparation: 4-(-methylnitrosamino)-1-(3-pyridyl)-butanol (NNAL) (racNNAL, CAS No. 76014-81-8), 4-(methylnitrosamino )-4-(3-pyridyl)butyraldehyde (NNA) (CAS No. 64091-90-3), 4-(methyl-d3-nitrosoamino)-1-(3-pyridyl)-1-butan Aldehydes (NNA-methyl-d3).

[0027] (1) Standard curve establishment:

[0028] Using acetonitrile as solvent, prepare NNAL, NNA and NNA-methyl-d3 standard single standard solutions with a concentration of 1 μg / mL, retaining four significant figures; using acetonitrile as solvent, prepare NNAL, NNA and NNA according to Table 2 -The mixed standard solution of methyl-d3; With the ratio of the concentration of NNA in the HPLC-MS-MS chromatogram and the concentration of NNA-methyl-d3 as abscissa, the quantitative ion pair peak area of ​​NNA in the chromatogram and NNA -The ratio of quantitative ion to peak area of ​​methyl-d3 is ordinate, establishes the stan...

Embodiment 2

[0037] The mensuration of NNAL and NNA in the shredded tobacco sample of embodiment 2

[0038] Repeat Example 1 to establish a standard curve and test samples, with the following differences: Accurately weigh 2.0 g of shredded tobacco into a 50 mL Erlenmeyer flask with a stopper, add 20 μL (1 ng / mL) of NNA-methyl-d3 solution, add 10 mL Ammonium formate aqueous solution with a concentration of 10mmol / L was shaken at room temperature for 20 minutes, the supernatant was taken, passed through a 0.2μm aqueous phase filter membrane, and detected by HPLC-MS-MS. Using the standard solution working curve of NNAL and the standard solution working curve of NNA to calculate the NNAL and NNA in the shredded tobacco sample, and then convert the contents of NNAL and NNA in the shredded tobacco sample to be 5.78ng / g and 10.46ng / g, respectively.

Embodiment 3

[0039] Example 3 Determination of NNAL and NNA in Total Particulate Matter of Cigarette Mainstream Smoke

[0040]Repeat Example 1 to establish a standard curve and sample detection, with the following differences: 20 cigarettes were smoked under standard smoking conditions, and 20 μL (1ng / mL) NNA-methyl-d3 solution, then add 14mL of dichloromethane and shake (45min, 160rpm) to extract. After the extract was evaporated to dryness, it was reconstituted with 500 μL of dichloromethane, and 1 mL of 0.1 mol / L HCl solution was added, vortexed to mix, and then left to separate layers. The upper aqueous phase was transferred to a clean glass bottle, and 120 μL of 1 mol / L NaOH solution was added to The sample was purified on a Waters Oasis HLB solid-phase extraction cartridge activated with 2 mL of methanol and 2 mL of water respectively, rinsed with 2 mL of 5% methanol aqueous solution, and finally eluted with 2 mL of methanol. The eluate was evaporated to dryness and dissolved in 10...

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Abstract

The invention discloses a method for detecting NNAL (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol) and NNA in cut tobacco and cigarette smoke. The method comprises the steps: preparing a mixed standard solution containing NNAL, NNA and NNA-methyl-d3, and respectively establishing standard solution working curves of NNAL and NNA by adopting an internal standard method; and then adding an NNA-methyl-d3 solution in a sample, adding an extraction solution, oscillating at a room temperature, collecting supernate, and performing HPLC-MS-MS (High Performance Liquid Chromatography-Mass Spectrometry) detection. The method has the advantages of low detection limit, good stability, rapidness and accuracy, and the like; a detection result is influenced by a subjective judgment factor a little, and thus the method is easy to popularize and apply.

Description

technical field [0001] The invention belongs to the technical field of tobacco chemical inspection, and in particular relates to a method for detecting the contents of NNAL and NNA in shredded tobacco and cigarette smoke. Background technique [0002] Tobacco-specific nitrosamines (TSNAs) are produced by nitrosation of tobacco endogenous alkaloids with nitrate and nitrite, and only exist in tobacco, tobacco products and cigarette smoke. In recent years, as smoking and health issues have attracted widespread attention, the research on various harmful chemical components in smoke has become increasingly in-depth at home and abroad. According to reports, eight tobacco-specific nitrosamines have been identified from tobacco leaves or cigarette smoke, including: N-nitrosonornicotine (NNN), 4-(methylnitrosamine)-1-( 3-pyridyl)-1-butanone (NNK), N-nitrosobasine (NAB), N-nitrosoannicotine (NAT), 4-(methylnitrosamino)- 1-(3-pyridyl)-1-butanol (NNAL), 4-(methylnitrosamino)-4-(3-pyri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 段焰青夏建军者为王文元蒋举兴党立志陈兴
Owner HONGYUN HONGHE TOBACCO (GRP) CO LTD
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