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.
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Authors
Dates
2020-04-21—Published
2019-05-20—Filed