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

A technology of cigarette mainstream smoke and normal phase liquid chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity, long analysis time, and difficulty in achieving accurate quantification, and achieve high sensitivity and short analysis time , the effect of improving the sensitivity

Active Publication Date: 2019-09-24
ZHENGZHOU TOBACCO RES INST OF CNTC
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Problems solved by technology

The problem of chiral chromatographic column-two-dimensional gas chromatography is that the analysis time is long; and the problem of chiral chromatographic column-liquid chromatography is that the sensitivity is low, and it is difficult to realize the low content of R-(+)-nicotine accurate quantification

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Smoke the balanced and screened cigarettes according to the standard conditions specified in YC / T29-1996, and use Cambridge filter to capture the particulate matter in the mainstream smoke of 5 cigarettes. Fold the Cambridge filter disc for trapping particulate matter into a 50 mL Erlenmeyer flask with a stopper, add 3 mL of 5.0% NaOH solution, let it stand for 15 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 30 min, and the supernatant was taken to pass through the organic phase filter membrane added 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: analysis by normal phase liquid chromatography-tandem mass spectrometry, the chromatographic column used is Daicel chiral chromatographic column CHIRALPAK ® IC, the size is 4.6 ...

Embodiment 2

[0027] Five typical cigarette samples were selected, and the content of nicotine optical isomers in the total particulate matter of mainstream cigarette smoke was determined according to the analysis method described in Example 1. The results are shown in Table 3.

[0028] Table 3: Contents of nicotine optical isomers in mainstream cigarette smoke (mg / cigarette)

[0029] Sample serial number S-(-)-nicotine R-(+)-nicotine 1# 0.1 0.003 2# 0.3 0.008 3# 0.6 0.019 4# 0.8 0.022 5# 1.1 0.033

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Abstract

A normal phase liquid chromatography-tandem mass spectrometry detection method of nicotine optical isomers in the mainstream smoke of cigarettes is characterized in that total particulate matters in smoke are captured by a Cambridge filter, nicotine is extracted with NaOH solution and n-hexane, the separation of the nicotine optical isomers is realized by adopting chiral chromatography-normal phase chromatography, isopropanol is introduced by a post-column high pressure infusion pump and is shunted, and tandem mass spectrometry is combined to carry out analysis. The method has the following advantages: 1, the nicotine optical isomers in the mainstream smoke of cigarettes are analyzed through adopting the normal phase liquid chromatography-tandem mass spectrometry; 2, the isopropanol is introduced by the isopropanol and is shunted to compensate the volume of a polar solvent entering a mass spectrometer, reduce the volume of a non-polar solvent and improve the ionization efficiency, so requirements of the liquid chromatography-tandem mass spectrometry are met; and 3, the chromatographic resolution of S-(-)-nicotine and R-(+)-nicotine is higher than that of existing methods (the retention time difference is 1 min), and the analysis time is short (only 17 min).

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 detection method for nicotine optical isomers in mainstream cigarette smoke, mainly a Cambridge filter Collect the total particle phase of cigarette mainstream smoke, extract nicotine on the filter with NaOH solution-n-hexane, use chiral chromatography column to separate nicotine optical isomers, introduce isopropanol into the high-pressure infusion pump behind the column and split the flow, combined with tandem mass spectrometry. 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. The two have completely different metabolic mechanisms and physiological characteristics, and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
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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