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METHOD OF DETERMINING POLYCYCLIC AROMATIC HYDROCARBONS IN SOILS AND BOTTOM SEDIMENTS

机译:测定土壤和底泥中多环芳烃的方法

摘要

FIELD: chemistry.;SUBSTANCE: invention relates to analytical chemistry and can be used in environmental control of various types of soil and bottom deposits for content of polyaromatic hydrocarbons (PAH). Method for chromatography-mass-spectrometric determination of PAH in a mode of monitoring preset ions in samples of soil and bottom sediments using a technique of dispersion liquid-liquid microectraction (DLLME) with preliminary extraction of PAH from solid samples into acetonitrile, in which at the stage of extraction of analytes from solid samples with weight 0.5 - 1 g into acetonitrile with volume of 500 mcl, using an ultrasonic treatment for 5 minutes, after which it is centrifuged for 10 minutes at rate of 10,000 rpm, the obtained supernatant is decanted, added with 3 ml of water and 550 mcl of a DLLME mixture consisting of 50 mcl of chloroform and 500 mcl of acetonitrile, obtained three-component system is shaken for 1 minute, centrifuged for 10 minutes at 3,000 rpm, and obtained extract is chromatographed, using a capillary column ZB-5ms with length of 60 m, an inner diameter of 0.25 mm with a graft phase of 5 % -polysilinyl-95 % -dimethylpolysiloxane with a film thickness of 0.25 mcm and a monocupernal mass spectrometer detector "Shimadzu GCMS-QP2020".;EFFECT: invention provides high selectivity, sensitivity of determination and increase in the amount of substances determined by optimizing sample preparation conditions and using a GC-MS analysis method.;1 cl, 2 tbl, 3 dwg
机译:发明领域本发明涉及分析化学,并且可以用于环境控制各种类型的土壤和底部沉积物中的聚芳烃(PAH)的含量。液相色谱-质谱法测定土壤和底部沉积物样品中的预设离子的方法是使用分散液-液微萃取(DLLME)技术,将固体样品中的多环芳烃初步提取为乙腈,其中从重量为0.5-1 g的固体样品中提取分析物到体积为500 mcl的乙腈中,使用超声波处理5分钟,然后将其以10,000 rpm的速度离心10分钟,然后倾析获得的上清液加入3 ml水和550 mcl的DLLME混合物(由50 mcl的氯仿和500 mcl的乙腈组成),振摇1分钟,以3,000 rpm离心10分钟,并将获得的萃取液进行色谱分离使用毛细管柱ZB-5ms,长度为60 m,内径为0.25 mm,接枝相为5%-聚甲硅烷基-95%-二甲基聚硅氧烷,膜厚为0。 25 mcm和单杯质谱检测器“ Shimadzu GCMS-QP2020”。效果:本发明通过优化样品制备条件和使用GC-MS分析方法,提供了高选择性,测定灵敏度和增加了所测定的物质量。1 cl,2 tbl,3 dwg

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