FIELD: medicine.
SUBSTANCE: fresh urine sample 10 cm3 is centrifuged at 2000 rpm for 10 min. An upper layer 1 cm3 is sampled for solid-phase extraction by sequential transmission under vacuum through a cartridge with Oasis HLB sorbent in proportions 1 thereof in 1 cm3, methylene chloride 1 cm3 in acetonitrile (1:10), distilled water 1 cm3, urine 1 cm3, distilled water 1 cm3, 50% aqueous acetonitrile 0.2 cm3. The cartridge is dried in air flow by a vacuum pump. Then the cartridge with the sorbent is transferred into a collection vessel (a weighing vessel) and passed through a sorbent of 100% methylene chloride 1.0 cm3. Extraction rate is 1 cm/min. An aliquot portion of the prepared extract is collected and chromatographed in Agilent series 1200 liquid chromatograph with a fluorimeter detector. Extraction rate (flow rate) is 1.5 cm3/min. An aliquot portion of the prepared extract is collected and chromatographed in Agilent series 1200 liquid chromatograph with a fluorimeter detector on a column 4.6×150 mm with Zorbax Eclipse XDB-Cis sorbent at column temperature 28°C, acetonitrile mixed with water is used as a movable phase at flow rate 1.5 cm3/min and optimised elution in a gradient mode, namely: 2.5 min supply of the movable phase consisting of 60 vol. % acetonitrile and 40 vol. % water, increase of acetonitrile 60 vol. % to 90 vol. % for 9.5 min, increase of acetonitrile 90 vol. % to 100 vol. % for 8 min, 4.5 min supply of 100% acetonitrile, decrease of acetonitrile to 60% for 2.5 min, supply of 60% acetonitrile for 5 min to balance the column. Excitation wave length of the fluorimeter detector made 265 nm, and emission wave length - 412 nm.
EFFECT: high sensitivity of the method combined with selectivity and availability for routine analyses.
3 cl, 5 tbl
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Authors
Dates
2012-11-10—Published
2011-10-20—Filed