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Automatic detection method of benzophenone and 4-methylbenzophenone in electronic cigarette liquid

A methyl benzophenone, automatic detection technology, applied in measurement devices, instruments, scientific instruments and other directions, can solve the problems of target concentration changes, poor precision, inaccurate measurement results, etc., to reduce differences and accuracy. error, avoiding long instrument waits, solvent consumption and the effect of less sample volume

Active Publication Date: 2018-05-18
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Benzophenone and 4-methylbenzophenone are intermediates of organic pigments, medicines, spices, and pesticides, and are irritating. The European Union (EC) No 19 / 2007 regulation stipulates that 4-methyl Benzophenone and benzophenone migration should not exceed 0.6 μg / g in total, but e-cigarette products lack supervision and quality is uneven, and benzophenone and 4-methylbenzophenone have been detected in some e-cigarette liquids Excessive ketone levels
[0004] At present, the analysis methods of benzophenone and 4-methylbenzophenone in the literature focus on the detection of instrumental analysis, and there are few studies on pretreatment. The pretreatment of benzophenone and 4-methylbenzophenone Most of the processing is manual offline processing, that is, solvent extraction is added to the sample, and the extract is taken into the instrument for analysis. However, manual pre-processing is not suitable for the general survey analysis of large-scale samples. The pre-processing human factors introduce large deviations and large system errors. Poor precision; when a large number of samples are analyzed, there will be a long waiting time before sample injection, and the solvent is volatile, which will cause the concentration of the target to change, and the measurement results will be inaccurate

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  • Automatic detection method of benzophenone and 4-methylbenzophenone in electronic cigarette liquid

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Experimental program
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Embodiment 1

[0027] 1. Pretreatment of the sample to be tested: add about 500 μL of e-cigarette liquid to the sample tray chromatography bottle, and make the front sampling tower add 0.5 mL of water to the sample; add 0.5 mL of dichloromethane to the sample; Sample tower Add 50 uL of 4-fluorobenzophenone internal standard to the sample; mix the sample at 1500 RPM for 1 min; wait for 5 min; move the sample vial to the front sampling tower; remove the lower dichloromethane phase 1 μL into GC-MS detection.

[0028] 2. GC-MS analysis conditions: Inlet temperature: 270°C; Injection volume: 1µL; Split ratio 10:1; Carrier gas: Helium, constant flow rate 1mL / min; Chromatographic column: DB-5MS, specification 30m ×0.25mm×0.25μm; temperature program: start at 100°C, keep for 2 minutes, increase to 230°C at a rate of 20°C / min, and keep for 5 minutes. Ionization method: EI; transfer line temperature: 280°C; ion source temperature: 230°C. Scanning method: SIM, the quantified ion of benzophenone is 10...

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Abstract

The invention discloses an automatic detection method of benzophenone and 4-methylbenzophenone in electronic cigarette liquid. The automatic detection method is characterized by directing by combiningpretreatment automation of an electronic cigarette sample with online gas chromatography-mass spectrum, i.e., directly putting the electronic cigarette sample in a chromatographic bottle, then setting the adding amounts of water, dichloromethane and internal standard, automatically adding by an instrument, carrying out volution, and online detecting the dichloromethane in the lower layer in a gaschromatography-mass spectrometer. Compared with an existing detection method, the automatic detection method disclosed by the invention has the technical advantages that 1, a whole process of samplepretreatment and sampling is in automatic operation, the difference and the accuracy error which are generated while the sample is manually treated are reduced, the repeatability is high, and generalsurvey analysis results are reliable; consumption of a solvent and the sample is less, and the automatic detection method is more environment-friendly; the automatic detection method is fast and efficient and is suitable for general survey analysis of large-batch products, and 150 samples can be treated and analyzed at a time; 2, inaccuracy of a target object determination result caused by solventvolatilization before conventional off-line detection is avoided, sampling is immediately carried out after pretreatment of each sample, and a determination result is accurate and reliable.

Description

technical field [0001] The invention belongs to the technical field of electronic cigarette liquid determination, and in particular relates to an automatic detection method for benzophenone and 4-methylbenzophenone in electronic cigarette liquid. In this method, the e-cigarette liquid pretreatment is automated and combined with online gas chromatography-mass spectrometry detection, the pretreatment uses less solvent, the whole process is automated, and the accuracy and repeatability are good. Background technique [0002] Electronic cigarette (electrical cigarette, e-cigarette), also known as electronic nicotine delivery systems (ENDS), is an electronic device that delivers nicotine to the respiratory system by means of electronic heating. new way. E-cigarette liquid is mainly composed of nicotine, propylene glycol, glycerin or polyethylene glycol, and a small amount of flavor is added to prepare different flavors to meet the needs and hobbies of consumers. [0003] Benzop...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 秦亚琼王晓瑜刘绍锋杨松潘立宁樊美娟余晶晶蔡君兰王冰贾云祯张晓兵刘惠民
Owner ZHENGZHOU TOBACCO RES INST OF CNTC