Validation of a High-Performance Liquid Chromatography Method for the Online Determination of Phthalates in Water at a Trace Level

被引:0
|
作者
Grigorieva, T. A. [1 ]
Kuzmin, A. V. [1 ]
Gorshkov, A. G. [1 ]
机构
[1] Russian Acad Sci, Limnol Inst, Siberian Branch, Irkutsk 664033, Russia
关键词
priority phthalates; microextraction and online HPLC; UV detection; high-resolution mass spectrometry; Lake Baikal; SOLID-PHASE MICROEXTRACTION; ORGANIC-COMPOUNDS; ACID-ESTERS; PRECONCENTRATION; EXTRACTION;
D O I
10.1134/S1061934824700874
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A method for the determination of phthalates in water is validated. It includes the sorption of hydrophobic components of a sample on a liquid chromatography column and the separation of analyte concentrated by online reversed-phase HPLC: for the quantitative determination of priority phthalates (PPhs) in surface waters at a trace level; qualitative assessment of the ratio of stable carbon isotopes C-13/C-12 in the PPh composition. It is shown that there is no contribution of PPhs from the laboratory background to the measurement results. The limits of determination (0.15-0.22 mu g/L) and the accuracy of the determination (+/-delta = 10-20%) are found using online reversed-phase HPLC and the UV detection of the analytes. The boundary values for the C-13/C-12 isotope ratio are substantiated for a qualitative assessment of the results of measuring the Delta C-13 value in the structure of di(2-ethylhexyl) phthalate and its ingress into waters of Lake Baikal from biogenic and abiogenic sources is revealed. A procedure for determining PPhs by reversed-phase HPLC with online UV detection is tested in the field using a portable liquid chromatograph; the concentration ranges for di-n-butyl phthalate (from <0.15 to 1.6 mu g/L) and di(2-ethylhexyl) phthalate (from <0.22 to 1.6 mu g/L) in the coastal zone of Lake Baikal are evaluated.
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页码:1483 / 1490
页数:8
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