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Method for extracting and purifying benzo[a] pyrene in cigarette smoke

A technology for cigarette smoke and benzo, which is applied in the field of chemical detection, can solve the problems of long extraction processing time, easy to cause errors, and long time consumption, and achieve the effect of important industrial application and promotion value

Inactive Publication Date: 2012-10-31
CHINA TOBACCO GUANGDONG IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method stipulated in the national standard is that when analyzing trace BaP in cigarette smoke, firstly, the extract obtained by ultrasonic extraction is carried out on the filter with smoke particulate matter, and then the silica gel solid-phase extraction column is used for purification and enrichment treatment. GC / MS analysis not only takes a long time for the extraction process itself, but also the purification and enrichment process is cumbersome, time-consuming and prone to errors

Method used

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  • Method for extracting and purifying benzo[a] pyrene in cigarette smoke
  • Method for extracting and purifying benzo[a] pyrene in cigarette smoke
  • Method for extracting and purifying benzo[a] pyrene in cigarette smoke

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Experimental program
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Effect test

Embodiment 1

[0035] 1. Reagents

[0036] Cyclohexane, dichloromethane, and acetone were all chromatographically pure (CNW, Germany); standard substances (Sigma-Aldrich, USA): benzo[a]pyrene (purity 98.7%), deuterated benzo[a]pyrene (BENZO( A) PYRENE-D 12, 98 ATOM% D), the preparation of the standard solution uses cyclohexane (analytical grade, or above) as the solvent, and obtains the required concentration by serial dilution; silicon-magnesium adsorbent, chromatography silica gel, neutral alumina (60 ~100 mesh, Sinopharm Chemical Reagents), after high-temperature activation treatment before use (high-temperature activation with muffle furnace, 550°C, 30min); solid-phase extraction cartridge (Supecol LC-SI, 500 mg); cigarette sample (marketed purchase) specifications: length 84 mm, diameter 8 mm.

[0037] 2. Instruments

[0038] 7890A / 5975C Gas-Mass Spectrometer (Agilent, USA); ASE-300 Accelerated Solvent Extractor (DIONEX, USA); Concentration System EVAIII Rota vapor? R-215 with Vacuum...

Embodiment 2

[0065] Embodiment 2 The effect comparison of extraction and purification integrated sample pretreatment of the present invention and ultrasonic extraction method

[0066] The method of the present invention: integrated treatment of ASE extraction and purification: 5g of purifying agent (silicon-magnesium-type adsorbent) is first filled in the 34 mL extraction pool, the filter piece loaded with flue gas particles is put into the extraction pool, and a certain amount of internal Marker. The extraction parameters were set as follows: 100% cyclohexane; pressure 10.3 MPa; temperature 100 °C; heating time 5 min; static extraction time 3 min; static extraction cycle 2 times; purge volume 40%; purge time 60 s; continuous extraction 3 times. The three extracts were combined and concentrated under reduced pressure to about 0.5 mL, and transferred to a chromatographic vial for GC / MS analysis.

[0067] Comparative test (GB / T 21130-2007): Ultrasonic extraction-SPE purification: Accurat...

Embodiment 3

[0084] Example 3 Cigarette Smoke Sample Analysis

[0085] According to the sample pretreatment method and GC / MS detection conditions and methods and steps described in Example 2, the ASE-GC / MS method and the USE-SPE-GC / MS method are applied to several different commercially available Cigarette smoke samples were analyzed for benzo[a]pyrene (internal standard D12-BaP with a concentration of 160 μg / L), and the results are shown in Table 4. The BaP release measured by the ASE-GC / MS analysis method is consistent with the USE-SPE-GC / MS analysis (GB method), and the RSD (n=3) is not more than 3.1%, indicating that the method of the present invention is stable and reliable, and can meet the analysis requirements .

[0086] Table 4 Analysis results of different types of cigarette samples (n=3)

[0087]

[0088] The ASE-GC / MS method of the present invention integrates extraction and purification processes, and the processing time for a sample is about 45 minutes. Compared with t...

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Abstract

The invention discloses a method for extracting and purifying benzo[a] pyrene in cigarette smoke, belonging to the technical field of chemical detection. The method comprises the steps of: collecting a filter sheet of smoke particles in an extraction pool filled with a purifying agent in the bottom, adding an internal standard substance, and mixing extraction solutions after extracting, wherein the extraction parameters are as follows: a solvent is cyclohexane, the pressure is 10.3MPa, the temperature is 40-200 DEG C, the heating time is 5-9min, the static extraction time is 01-0min, the static extraction is circulated for 1-5 times, the purging volume is 40-150 percent, the purging time is 60-120s, and the extraction is continuously extracted for 2-5 min. The method is combined with a GC / MS detection condition specified in the national standard without largely modifying the GC / MS detection condition and equipment, can be implemented more accurately and reliably, conveniently and rapidly through slight modification on the basis of the traditional condition in a time and labor saving manner, and has an important industrial application and popularization value.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method for extracting and purifying benzo[a]pyrene in cigarette smoke. Background technique [0002] Benzo[a]pyrene (BaP for short) is a fused-ring aromatic hydrocarbon compound with five rings, and its molecular formula is C 20 h 12 , the molecular weight is 252.32. BaP is a carcinogen, teratogen, and mutagen, and its carcinogenic effect is significantly higher than that of other condensed aromatic hydrocarbons. It is one of the seven representative harmful components of cigarette smoke that are currently concerned. Fast and accurate detection of BaP in medium. [0003] The smoke components produced by the burning process of cigarettes are extremely complex. According to reports, more than 5,000 smoke components have been detected, and the amount of BaP is usually 5-40 ng / cigarette, and there are a lot of interfering substances. Therefore, how to eliminate inte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/14G01N30/02
Inventor 汪军霞吴君章韩冰胡静李峰
Owner CHINA TOBACCO GUANGDONG IND
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