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Method for determining the purity of nicotine by gas chromatography-mass spectrometry combined with gas chromatography

A gas chromatography mass spectrometry and gas chromatography technology, which is applied in the field of quality evaluation and determination of tobacco and tobacco products, can solve the problems of inability to distinguish nicotine and nornicotine, difficult formation of precipitates, interference with detection results, etc., and achieve reliable qualitative and quantitative results. , strong separation ability, good repeatability

Active Publication Date: 2016-08-24
YUNNAN TOBACCO QUALITY SUPERVISION MONITORING STATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can obtain more accurate results, but has certain limitations: the analysis time is longer; nicotine and nornicotine cannot be distinguished, and the measurement result is the sum of the two substances; when the solution contains inorganic salts such as ammonium salts, Precipitation is not easy to form and interferes with the test results

Method used

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  • Method for determining the purity of nicotine by gas chromatography-mass spectrometry combined with gas chromatography
  • Method for determining the purity of nicotine by gas chromatography-mass spectrometry combined with gas chromatography
  • Method for determining the purity of nicotine by gas chromatography-mass spectrometry combined with gas chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0045] (1) Materials and instruments:

[0046] (1) Reagents: hydrochloric acid (AR, Yantai Shuangshuang Chemical Co., Ltd.); silicotungstic acid (AR, Shanghai Reagent No. 2 Factory); isopropanol (chromatographically pure, TEDIA Company, Inc.); absolute ethanol (AR, Shanghai Reagent No. 1 Factory);

[0047] (2) Instruments: Motto-Q ultrapure water device (Millipore Company); AG204 electronic balance (sensitivity: 0.0001g, Swiss METTLER TOLEDO Company); blast constant temperature drying oven (101A-2, Shanghai General Experimental Instrument Factory) GC / MS (5975, Agilent Company); GC (7890, Agilent Company); Quantitative Liquid Adder (Germany Brand Company); Pipette Gun (Tripette Company).

[0048] (2) Preparation of samples and determination of nicotine purity:

[0049] (1) Preliminary determination of the purity nic% of nicotine by GC / MS method

[0050] A. Sample preparation: Dilute nicotine sample A (long-term sample) 100 times with isopropanol as the sample to be tested, t...

Embodiment 2

[0095] Repeat the process of Example 1, select another nicotine sample B (newly prepared sample), prepare 7 parts of diluted solutions, and measure its nicotine content with GC-MS method, the spectrogram is as follows figure 2 Shown, measured value is successively 99.53%, 99.53%, 99.46%, 99.64%, 99.51%, 99.56%, 99.58%, measured average value is 99.54%, SD is 0.06; Its water content and its average value and GC / MS -Results of nicotine purity (NIC%) determined by GC method are shown in Table 1 and Table 2 respectively.

Embodiment 3

[0097] Repeat the process of Example 1, select another nicotine sample C (a long-standing sample), and prepare 4 parts of diluted solutions, and measure its nicotine content by GC-MS method, and the spectrogram is as follows: image 3 As shown, the measured values ​​were 99.05%, 99.01%, 99.06%, and 99.01% in turn, the measured average value was 99.03%, and the SD was 0.03. The water content and its average value and the results of nicotine purity (NIC%) determined by GC / MS-GC are shown in Table 1 and Table 2 respectively.

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Abstract

The invention discloses a method for measuring nicotine purity combination of a gas chromatography-mass spectrometry method and a gas chromatographic method. The purity of the nicotine is preliminarily measured by use of the GC-MS method, next, the moisture content in the nicotine is measured by use of the GC method, and finally, the accurate purity of the nicotine is obtained by virtue of correction according to a correction formula NIC%=nic%*(100%-wat%). Compared with a silicotungstic acid weight method, the method has the characteristics of being simple and convenient, fast, easy to operate and good in repeatability. The method is high in nicotine detection specificity, and is not affected by other impurities, in particular alkaline impurities (alkaloid and inorganic bases), in the sample; during purity detection on the nicotine sample, in particular a sample which is arranged for a long time and is high in impurity content, the method is simple and convenient to operate, and high in separation capacity, and the qualitative and quantitative results are reliable.

Description

technical field [0001] The invention belongs to the technical field of quality evaluation and measurement of tobacco and tobacco products, and in particular relates to a method for measuring the purity of nicotine by combining gas chromatography-mass spectrometry with gas chromatography. technical background [0002] Nicotine (also known as nicotine, English name nicotine), has the effect of excitatory and then paralyzed on the autonomic and central nervous system. It is one of the important components of tobacco and tobacco products, and it is also a measure of the quality control of tobacco and tobacco products. Important indicators. At the same time, nicotine can be used in the production of medicines, biological pesticides, cigarette additives, catalysts and other products. Therefore, the analysis of nicotine, especially the determination of nicotine purity, is not only related to the quality control of tobacco and tobacco products, but also has great significance for t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 蔡洁云李雪梅李海燕马慧宇陈新瑞王惠平
Owner YUNNAN TOBACCO QUALITY SUPERVISION MONITORING STATION