Method for determining six aromatic amine compounds in cigarette mainstream smoke by using online SPE/LC-MS/MS

A technology of cigarette mainstream smoke and aromatic amines, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as human error, tedious and time-consuming processing, achieve high precision, reduce sample analysis interference, and reduce pollution.

Active Publication Date: 2017-01-04
中国烟草总公司山东省公司
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Problems solved by technology

[0006] The purpose of the present invention is to provide an online solid-phase extraction-liquid chromatography-tandem mass spectrometry technology for the determination of the content of the main stream smoke of cigarettes in view of the shortcomings of tedious and time-consuming sample pretreatment and easy introduction of human error in the existing aromatic amine compound detection technology. 6 Methods of Aromatic Amines

Method used

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  • Method for determining six aromatic amine compounds in cigarette mainstream smoke by using online SPE/LC-MS/MS
  • Method for determining six aromatic amine compounds in cigarette mainstream smoke by using online SPE/LC-MS/MS
  • Method for determining six aromatic amine compounds in cigarette mainstream smoke by using online SPE/LC-MS/MS

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Experimental program
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Effect test

Embodiment 1

[0032] 1. Sample preparation

[0033] The balanced and screened cigarettes are smoked according to the standard conditions specified in ISO 3308:2000, and 4 Cambridge filters (φ44mm) are used to capture the particulate matter in the mainstream smoke of 20 cigarettes (each Cambridge filter captures 5 Particulate matter in the mainstream smoke of cigarettes); an absorption bottle pre-filled with 25 mL of 2% formic acid solution is connected to the back of the trap through a hose to collect gaseous matter.

[0034] Remove the absorption bottle that collects the gas phase and add 0.25 mL mixed internal standard (d 9 -O-toluidine, d 3 -O-anisidine, d 6 -2,6-Dimethylaniline, d 7 -1-Aminonaphthalene and d 9 -4-aminobiphenyl), mix well, and directly enter Online SPE / LC-MS / MS analysis.

[0035] Fold the Cambridge filter with 20 cigarette mainstream smoke particles into a 250mL conical flask, add 1.0mL mixed internal standard and 100mL 2% formic acid solution (extract solution), and ultrasonic...

Embodiment 2

[0070] The Kentucky reference cigarette 3R4F was pumped in accordance with the standard conditions specified in ISO 3308:2000, and the particulate matter of 5 cigarettes was collected per Cambridge filter, and the gaseous matter was collected in an absorption bottle containing 25 mL of 2% formic acid solution.

[0071] Then, the sample processing and analysis were performed according to the steps and conditions described in Example 1. Six parallel experiments and five-day determinations were performed. The relative standard deviations of the determination of each compound were between 2.50-5.52% and 2.24-6.69, indicating that the method has good reproducibility and stability.

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Abstract

The invention discloses a method for determining six aromatic amine compounds in cigarette mainstream smoke by using online SPE / LC-MS / MS. It uses the Cambridge filter and an absorption bottle containing 2% formic acid solution to capture the aromatic amine compounds in the main cigarette smoke particle and gas phase matters, respectively, ultrasonically extracting the filter by 2% formic acid solution, adding interior labels into the two solutions and determining the six aromatic amine compounds by online SPE / LC-MS / MS, including o-toluidine, 2,6-dimethylaniline, o-anisidine, 1-aminonaphthalene, 2-aminonaphthalene and 4-aminobiphenyl. The method has the advantages of simplifying the sample pretreatment process and extracting with the formic acid solution to reduce the pollution. The two-dimensional in-line solid-phase extraction composed of the cationic column and the reversed-phase C18 column is used to purify the sample to be tested and the purification effect is good; each target is quantitatively analyzed using their specific internal standard, effectively reducing the matrix effect.

Description

Technical field [0001] The invention belongs to the technical field of analysis and testing of related components of cigarette smoke emissions, and specifically relates to a method for determining 6 aromatic amine compounds in mainstream cigarette smoke by applying online solid phase extraction-liquid chromatography-tandem mass spectrometry technology, including o-methyl Alkylaniline, 2,6-dimethylaniline, o-anisidine, 1-aminonaphthalene, 2-aminonaphthalene and 4-aminobiphenyl. Background technique [0002] As important organic synthesis raw materials and intermediates, aromatic amine compounds are widely used in the industrial production of drugs, pesticides, azo dyes, plastics, and rubber. In addition, people have detected various aromatic amines from various environmental substances such as air, discharged wastewater, food additives, cosmetics, etc. Aromatic amine compounds can enter the human body through breathing, ingestion or skin contact, and can cause damage to the human...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 纪立顺别振英朱友陈玉松蔚亦沛陆伟罗旭刘敏
Owner 中国烟草总公司山东省公司
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