ABSTRACT
An analytical method based on high performance liquid chromatography tandem mass spectrometry has been developed for the simultaneous determination of 20 anti-obesity drugs ( fenfluramine, phenylpropanolamine, sibutramine, sertraline, rimonabant, bupropion, citalopram, fluoxetine, benfluorex, topiramate, zonisamide, caffeine, phenolphthalein, emodin, indapamide, bumetanide, torasemide, triamterene, orlistat, phenformin). that were extracted from various weight-loss functional foods by ethanol-acetone(7:3, V/V)and purified by primary secondary amine (PSA) and octadecyltrimethoxysilane(ODS) under ultrasonication. The analysis was carried out on HPLC-MS /MS by electrospray ionization using multiple reaction monitoring after the chromatographic separation on Waters Atlantis T3 (3 μm, 150 mm × 2. 1 mm) column. Identification was achieved by the retention time and the ion ratio, quantification was done by the external standard method. The limits of detection for the appetite suppressants were 0. 05-3. 0 mg/kg. The mean recoveries at the three spiked levels were 67 . 1%-101 . 4%, with the intra-day precision less than 10%and the inter-day precision less than 15%. The method is reliable, accurate, reproducible and suitable for the determination of the anti-obesity drugs in different weight-loss functional foods.
ABSTRACT
A comprehensive analytical method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of active components and anti-diabetic) drugs in propolis health foods. The samples were extracted by ultrasound extraction with methanol). The insoluble residue of extract was removed by freeze-centrifuging. The analysis was performed on an ACQUITY UPLC C_(18)) column(50 mm ×1 mm, i.d., 1.7 μm) utilizing a gradient elution profile and a mobile phase of 0.3% formic acid in water and acetonitrile. The analytes were detected using an electro spray ionization tandem mass spectrometry with multiple reaction monitoring. Qualitative and quantitative analysis was based on the peak area of the parent ion and two fragment ions. The LOD and LOQ level for 14 active components ranged from 0.7 mg/kg to 42.0 mg/kg and 2.2 mg/kg to 140 mg/kg respectively, and recoveries were 77.8%-113.6%, with the intra- and inter-day precision less than 15%. The LOD and LOQ level for 9 anti-diabetics) ranged from 0.1 mg/kg to 0.9 mg/kg and 0.3 mg/kg to 2.5 mg/kg respectively, and recoveries) were 79.3%-108.5%, with the intra- and inter-day precision less than 15%. The method is simple) and sensitive, and can be used for quality control of propolis.
ABSTRACT
An analytical method based on high performance liquid chromatography tandem mass spectrometry has been developed for the determination of 11 appetite suppressants (fenfluramine,phenylpropanolamine,sibutramine,sertraline,rimonabant,bupropion,citalopram,fluoxetine,benfluorex,topiramate,zoni-samide). Various weight-loss functional foods were extracted under accelerated solvent extraction and separated on Waters Atlantis T3( 150 mm×2.1 mm,3μm) column. The analysis was carried out on HPLC-MS/MS by electrospray ionization using multiple reaction monitoring. Identification was achieved by ihe retention time and the ion ratio,quantification was done by the external standard curves. The limits of detection for the appetite suppressants were 0.05-4.0 mg/kg. The mean recoveries at the three spiked levels(low,middle,high) were 78.3% - 103. 6% ,with the intra-day precision less than 12% and the inter-day precision less than 15%. The method is reliable,sensitive,reproducible,and adapts to the determination of the appetite suppressants in different weight-loss functional foods.