A method for the detection of nicotine optical isomers in snus by normal phase liquid chromatography-tandem mass spectrometry

A normal-phase liquid chromatography and optical isomer technology, applied in the field of measurement technology research, can solve the problems of long analysis time and low sensitivity, and achieve the effect of short analysis time, high sensitivity and high chromatographic separation

Active Publication Date: 2019-08-30
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • 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

Method used

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  • A method for the detection of nicotine optical isomers in snus by normal phase liquid chromatography-tandem mass spectrometry
  • A method for the detection of nicotine optical isomers in snus by normal phase liquid chromatography-tandem mass spectrometry
  • A method for the detection of nicotine optical isomers in snus by normal phase liquid chromatography-tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Pretreatment of different types of snout samples:

[0027] Pouched wet snuff: cut open the mouth of the bag, take out the cut tobacco inside, cut the bag into pieces, and mix with the cut tobacco in the mouth.

[0028] Sulfur-containing smoky: Take slurried smoky and pulverize directly.

[0029] Gum-based snout: Take the gum-based snout and grind it into a sheet with a grinding bowl, and then cut it with scissors.

[0030] (2) Extraction of nicotine in snout: Weigh 0.3g of pretreated snout sample, add 2 mL of 5.0% NaOH solution, let it stand for 20 min, and accurately add racemic d 3 -20 mL n-hexane solution of nicotine internal standard, racemic d 3 -Nicotine concentration is 5mg / mL, ultrasonic extraction for 30 minutes, take the supernatant organic phase filter membrane, add 2.0 g of anhydrous sodium sulfate to the organic phase filter membrane, and the purified sample solution is sent to normal phase liquid chromatography-tandem Mass Spectrometry.

[0031] (3) Instrumenta...

Embodiment 2

[0033] Two typical samples of bagged moist snuff, chemical-containing snuff, and gum-based snuff were selected, and the content of nicotine optical isomers in snuff was determined according to the analysis method described in Example 1. The results as shown in Table 3.

[0034] Table 3: The content of nicotine optical isomers in snuff (mg / g)

[0035] Sample serial number S-(-)-Nicotine R-(+)-nicotine Bags of wet snuff 15.60.011 Bags of wet snuff 213.70.037 Containing Sulfur 14.80.014 Containing Sulfur 26.90.017 Gum-based snout 19.80.027 Gum-based snout 2 7.60.017

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Abstract

Provided is a method for detecting nicotine optical isomers in buccal tobacco by using normal-phase liquid chromatography-tandem mass spectrometry. The method is characterized in that firstly, nicotine in the buccal tobacco is extracted, a chiral chromatographic column is adopted to separate the nicotine optical isomers, a post-column high-pressure infusion pump introduces isopropanol and conducts splitting, assay determination is conducted in combination with the tandem mass spectrometry, and therefore the sensitive detection and the separation of S-(-)-nicotine and R-(+)-nicotine are achieved. The method has the advantages that by the adoption of the post-column high-pressure infusion pump for introducing the isopropanol and conducting the splitting, the volume of a non-polar solvent added into a mass spectrometer is reduced, the volume of the polar solvent isopropanol is compensated at the same time, the ionization efficiency is improved, so that requirements of liquid chromatography-tandem mass spectrometry analysis are met, and the sensitivity of the analysis is improved; compared with current methods, the chromatographic separation degree of the two nicotine optical isomers is high, wherein retention time difference between the two nicotine optical isomers is one minute; the analysis time is short, wherein only seventeen minutes are needed.

Description

Technical field [0001] The present invention belongs to the research on the separation, analysis and detection technology of chiral isomers in complex samples, and specifically relates to a method for analyzing optical isomers of nicotine in snout smoke by normal phase liquid chromatography-tandem mass spectrometry, mainly for different types The nicotine is extracted from the nicotine sample, and the chiral chromatography column is used to separate the optical isomers of nicotine. The post-column high-pressure infusion pump introduces isopropanol and splits the flow. Combined with tandem mass spectrometry, the nicotine is extracted. Separation and sensitive detection of S-(-)-nicotine and R-(+)-nicotine. Background technique [0002] Sulfur is a smokeless tobacco product used through the oral cavity. It is composed of tobacco powder / shredded tobacco / tobacco extract and added inorganic salts, flavors, moisture, moisturizers and other ingredients. The product forms include America...

Claims

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Application Information

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Patent Type & Authority Patents(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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