METHOD FOR QUANTITATIVE DETERMINATION OF BENSULTAP IN MEDICINAL VEGETAL RAW MATERIALS

摘要

The invention relates to biology, ecology, toxicological and sanitary chemistry, and can be used to control the content of bensultap in medicinal vegetal materials. The medicinal vegetal material is crushed, treated with a mixture of acetonitrile-dichloroethane-ethyl acetate 6:2:2 by volume, taken at four times material quantity by weight, the extract is dehydrated, evaporated, the residue is dissolved in acetone, chromatographed in a macro column 49010 mm in size, filled with 10 g of Merk silica gel 40/63 , first passing 20 ml of hexane through it, and then eluting with a solvent mixture of diethyl ether-hexane in a ratio of 8:2 by volume, the eluate is collected in 2 ml fractions, eluate fractions 18 to 24 are joined, the eluent is evaporated, the residue is dissolved in dichloromethane, and bensultap is detected by gas chromato-mass spectrometry technique in a capillary column with 5% phenyl-95% methyl polysiloxane, using a helium carrier gas supplied at a rate of 0.6 ml/min and a mass selective electron impact detector; the initial temperature of the column is 70°C, it is held for 3 min, increased at a rate of 20°C per minute to 290°C and maintained for 16 min, the temperature of the injector is 250°C, that of quadrupole is 150 C, that of the detector interface is 300°C; mass spectrum is recorded by the total ion current, and the amount of bensultap is calculated from the area of its chromatographic peak. The method provides increased sensitivity.