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Positive-phase liquid chromatogram-tandem mass spectrum detection method for nicotine optical isomers in tobacco and tobacco products

A technology of normal phase liquid chromatography and optical isomers, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of long analysis time, difficulty in accurate quantification of R-(+)-nicotine, and low sensitivity. To achieve the effect of short analysis time, improved sensitivity and high sensitivity of the method

Active Publication Date: 2017-07-14
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with chiral chromatographic column-two-dimensional gas chromatography is that the analysis time is long; while the problem with chiral chromatographic column-liquid chromatography is low sensitivity
Existing methods are difficult to achieve accurate quantification of R-(+)-nicotine with low content

Method used

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  • Positive-phase liquid chromatogram-tandem mass spectrum detection method for nicotine optical isomers in tobacco and tobacco products
  • Positive-phase liquid chromatogram-tandem mass spectrum detection method for nicotine optical isomers in tobacco and tobacco products
  • Positive-phase liquid chromatogram-tandem mass spectrum detection method for nicotine optical isomers in tobacco and tobacco products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Pretreatment of tobacco leaf samples: Accurately weigh 0.30 g cut tobacco, add it into a 50 mL Erlenmeyer flask with a stopper, add 2 mL of 5.0% NaOH solution, let it stand for 10 min, and accurately add d 3 - 20 mL of nicotine racemate in n-hexane, racemic d 3 -The concentration of nicotine was 5 mg / mL, ultrasonically extracted for 15 min, the supernatant was passed through the organic phase filter membrane with 2.0 g of anhydrous sodium sulfate in the syringe, and the filtrate was analyzed by normal phase liquid chromatography-tandem mass spectrometry.

[0025] (2) Instrumental analysis conditions: Normal phase liquid chromatography-tandem mass spectrometry is used for analysis, and the chromatographic column used is Daicel chiral chromatographic column CHIRALPAK ® IC, the size is 4.6 mm×250 mm, i.d. 5 µm; column temperature: 30 o C; mobile phase A: n-hexane containing 0.1% diethylamine, mobile phase B: isopropanol; 95%A+5%B isocratic elution; flow rate 1.0 mL / m...

Embodiment 2

[0027] Five kinds of tobacco leaf samples were selected, and the content of nicotine optical isomers in the samples was determined according to the analysis method described in Example 1, and the results are shown in Table 3.

[0028] Table 3 Contents of nicotine optical isomers in tobacco leaf samples (mg / g)

[0029] Sample serial number S-(-)-nicotine R-(+)-nicotine 1# 14.30 0.036 2# 16.32 0.049 3# 19.60 0.045 4# 18.30 0.049 5# 18.42 0.052

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Abstract

The invention relates to a positive-phase liquid chromatogram-tandem mass spectrum detection method for nicotine optical isomers in tobacco and tobacco products. The positive-phase liquid chromatogram-tandem mass spectrum detection method is characterized in that nicotine in tobacco leaves is extracted by a NaOH (sodium hydroxide) solution and n-hexane, the nicotine optical isomers are separated by a chiral chromatographic column, a post-column high pressure liquid output pump is used for introducing isopropyl alcohol and separating flow, and the tandem mass spectrum is used for analyzing, so as to complete the separation and sensitive detection of S-(-)-nicotine and R-(+)-nicotine in the tobacco and tobacco products. The positive-phase liquid chromatogram-tandem mass spectrum detection method has the characteristics and beneficial effects that the post-column high pressure liquid output pump is used for introducing isopropyl alcohol and separating flow, so that the amount of non-polarity solvent entering mass spectrum is reduced, the amount of isopropyl alcohol of polarity solvent is compensated, the ionizing efficiency is improved, the requirement of liquid chromatogram-tandem mass spectrum analysis is met, and the analysis sensitivity is improved; compared with the prior art, the chromatographic resolution of the two types of nicotine optical isomers is high, and the difference of retention times is 1min; the analysis time is short, and is only 17min.

Description

technical field [0001] The invention belongs to the technical research on the separation, analysis and detection of chiral isomers in complex samples, and specifically relates to a normal phase liquid chromatography-tandem mass spectrometry method for analyzing nicotine optical isomers in tobacco and tobacco products, mainly using NaOH solution- The nicotine in tobacco leaves was extracted with n-hexane, and the optical isomers of nicotine were separated by chiral chromatographic column. The high-pressure infusion pump behind the column introduced isopropanol and split the flow. Combined with tandem mass spectrometry analysis, the separation of S in tobacco and tobacco products was realized. Separation and sensitive detection of -(-)-nicotine and R-(+)-nicotine. Background technique [0002] Nicotine is the most abundant alkaloid in tobacco and smoke, and is the main driving force for human smoking. Nicotine has two optical isomers, namely S-(-)-nicotine and R-(+)-nicotine....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 余晶晶蔡君兰王冰秦亚琼刘克建赵晓东薛聪刘绍锋张晓兵
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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