Method for simultaneously measuring 12 kinds of alkaloid in tobacco and tobacco products
A technology for tobacco products and alkaloids, applied in the field of physical and chemical analysis, can solve problems such as false positive results, unsatisfactory separation effect, and less research
Inactive Publication Date: 2017-10-24
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Problems solved by technology
However, the minor alkaloids in these studies are mainly concentrated on nornicotine, anatabine, pseudobasine, mesmin, etc., while there are fewer studies on other minor alkaloids
For example, the current literature reports that the determination of the number of alkaloids in tobacco is at most 8, using the GC-NCD method (Anal. Methods. 2012;4(7):2095-2100.) and the LC-MS / MS method (J. Chromatogr. Sci. 2015;53(10):1730-1736.), but the selectivity of GC-NCD method is not very good, it is prone to false positive results, and the detection limit of LC-MS / MS for some target objects is too high , and the separation effect is not ideal
Lisko et al. used GC-MS / MS to analyze alkaloids in tobacco (nornicotine, neonicotinoid, mesmin, pseudobasine, 2,3'-bipyridine), but there were only 5 targets (Anal . Chem. 2013;85(6):3380-3384.)
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Embodiment 1
[0073] 1. Instruments and reagents
[0074] Instruments: gas chromatography-mass spectrometry (Agilent 7890B-5977A, USA); SM450 linear smoking machine (Srulin, UK); AE163 electronic balance (sensitivity: 0.0001 g, Mettler, Switzerland); Talboys digital display Multi-tubular vortex mixer; centrifuge (3-30K, SIGMA).
[0075] Reagent consumables: nornicotine was purchased from alfa, the other 11 tobacco alkaloids were purchased from TRC, quinoline (alfa), nornicotine-2,4,5,6-d 4 (CDN Isotopes), 2,2'-bipyridine-d 8 (CDN Isotopes), methanol (DUKSAN, chromatographically pure), dichloromethane (DUKSAN, chromatographically pure), sodium hydroxide (Sinopharm, analytically pure), and water used was produced by a Milli-Q system (Milford, MA, USA).
[0076] 2. Sample pretreatment
[0077] Accurately weigh about 300 mg of tobacco sample into a 15 mL plastic centrifuge tube, then add 50 μL of internal standard stock solution and 2.0 mL of 5% sodium hydroxide solution, shake and mix well,...
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Abstract
The invention relates to a method for simultaneously measuring 12 kinds of alkaloid in tobacco and tobacco products and belongs to the technical field of physical and chemical analysis. The method includes the following steps that 1, alkaloid in the tobacco is dissociated out with a 5% sodium hydroxide water solution; 2, a dichloromethane / methyl alcohol mixed solution (V dichloromethane / V methyl alcohol=4:1) is used as an extracting agent for liquid-liquid oscillating extraction; 3, after room temperature standing, a lower-layer organic phase is taken and transferred into a chromatographic analysis bottle for GC-MS analysis. The adding standard recovery of the 12 kinds of alkaloid ranges from 83.36% to 111.88%, the precision degree is not higher than 7.93%, the method detection limit ranges from 0.025 microgram / gram to 0.620 microgram / gram, and the advantages of being easy and convenient to operate, high in flux, high in sensitivity, good in recovery and repeatability and the like are achieved.
Description
technical field [0001] The invention belongs to the technical field of physical and chemical analysis, and in particular relates to a method for simultaneously measuring 12 alkaloids in tobacco and tobacco products. Background technique [0002] Alkaloids refer to a class of organic compounds containing nitrogen heterocycles (excluding proteins, titanium, amino acids, ammonia, amino sugars, nucleotides, and nucleic acids) that exist in living organisms. They are generally alkaline and exhibit physiological activity. Alkaloids have a special status in tobacco and its products. It is not only an important quality factor of tobacco, but also specifies the characteristics of tobacco as a commodity. Nicotine accounts for more than 92% of the total alkaloids in tobacco. People smoke tobacco largely to obtain nicotine, so it is the most important alkaloid in tobacco. Its existence endows tobacco and its products with unique charm . In addition to nicotine, tobacco also contains o...
Claims
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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 韩书磊陈欢付亚宁刘彤李翔宇张洪非罗彦波庞永强韩雪侯宏卫胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT