Pretreatment method for benzo(a)pyrene collected in glass fiber filter paper

Abstract

The present invention discloses a pretreatment method of benzo (a) pyrene collected by glass fiber filter paper, first, glass fiber filter paper with the collected benzo (a) pyrene is cut, and put into a brown headspace sample bottle, then the headspace sample bottle is continued to be added with methanol as a desorption solvent, and then added with a certain amount of alumina, the alumina can absorb and purify interference impurities in a sample; the headspace sample bottle is sealed, and put into an ultrasound device with circulating cooling water for ultrasound desorption for a period of time; finally the headspace sample bottle is taken out, and put into a centrifuge for centrifuging for a period of time at a set rotational speed, and a supernatant is taken and expanded and analyzed by chromatography. The method has the advantages of simple and available appliances, closed pretreatment process, small outside world pollution, fast pretreatment speed, high benzo (a) pyrene desorption recycling efficiency and the like.

Description

technical field [0001] The invention relates to the technical field of analysis of benzo(a)pyrene content determination, in particular to a pretreatment method for benzo(a)pyrene collected through glass fiber filter paper. Background technique [0002] Benzo(a)pyrene, formula C 20 h 12 , is the most toxic and strong carcinogen among polycyclic aromatic hydrocarbons. The determination of polycyclic aromatic hydrocarbons, especially benzo(a)pyrene, in air and other environments is the focus of attention. At present, the determination of benzo(a)pyrene is generally firstly collected through glass fiber filter paper, and then transferred to a liquid solvent through steps such as elution and desorption, rinsing and filtration, concentration and enrichment, and then detected by chromatographic techniques. [0003] At present, there have been many researches on the pretreatment technology of benzo(a)pyrene collected by glass fiber filter paper. The earlier GB / T8971-1988 "Determi...

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Problems solved by technology

HJ 646-2013 "Gas Chromatography-Mass Spectrometry for the Determination of Polycyclic Aromatic Hydrocarbons in Ambient Air and Exhaust Gas Phase and Particulate Matter" was extracted by a Soxhlet extractor for up to 16 hours with a mixed solvent of ether / n-hexane. The extract was concentrated and passed through Purification by silica gel column and other methods takes a long time and the operation steps are cumbersome

GBZ / T 160.44-2004 "Determination of Polycyclic Aromatic Hydrocarbon Compounds in Air Toxic Substances in the Workplace" uses cyclohexane in a stoppered colorimetric tube for multiple ultrasonic extractions, and the extract is enriched by KD concentration or rotary evaporation. The operation steps complex

GB / T 15439-1995 "High Performance Liquid Chromatography for the Determination of Benzo[a]pyrene in Ambient Air" uses acetonitrile for ultrasonic extraction, and takes the supernatant for analysis, but because the glass fiber filter membrane is sheared during ultrasonication, it is difficult to Obtaining a clear supernatant can cause irreversible damage to the column

Zhou Jingbo (Determination of benzo(a)pyrene in ambient air by ultrasonic extraction high-performance liquid chromatography, Proceedings of the Annual Conference of the Chinese Society for Environmental Sciences (2012), 602-605) adopts the method of methanol ultrasonic desorption, and the filtrate is passed through a polymer Injection analysis after filtration of vinyl fluoride, although glass fiber filter debris can be avoided from entering the chromatographic column, it is difficult to avoid the influence of complex coexistence matrix in the sample on chromatographic separation

Zheng Hongyan (Determination of benzo(a)pyrene in the atmosphere by high performance liquid chromatography [J]. Chinese Public Health, 2005, 21(12): 1522-1523) used a disposable centrifuge tube with a cover for long-term ultrasound Elution, due to the loss of benzo(a)pyrene due to loose sealing, the recovery rate of standard addition is less than 90%

Researches such as Wang Chunhua (high performance liquid chromatography is determined 3_4_benzopyrene in asphalt smoke [J]. Environment and Occupational Medicine, 2007,24 (4): 443-445) etc. are also long-term Soxhlet extraction and rotary evaporation concentration steps complicated

That is to say, the current general pretreatment technology has problems such as cumbersome operation or low efficiency of desorption and recovery of benzo(a)pyrene.

[0004] CN104049053A discloses a pretreatment method for measuring benzopyrene in instant noodles, wherein it is recorded as a pretreatment extraction method for benzo(a)pyrene in instant noodle samples, which is not applicable to benzo(a)pyrene collected by fiber filter membranes. The pretreatment of pyrene; and CN103278595A discloses a special automatic detection equipment for benzopyrene, and CN201310163371.7 pays attention to a kind of detection equipment that combines sample processing and liquid chromatography, and does not involve the specific separation technical scheme of pretreatment

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