| At present,the official detection method issued by the State Food and Drug Administration,which has been unable to meet the actual regulatory needs,only received eight kinds of common weight loss drugs.Therefore,the establishment of a larger capacity detection method,which can simultaneously detect a variety of illegally added chemicals in health food,is very necessary.The probability added chemicals were selected according to the efficacy of drugs and side effects.In this subject,to develop detection method for the simultaneous screening and confirmation of 29 illegally added in slimming health food using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples(including slimming tea,slimming capsules,weight loss tablets)were in methanol ultrasonically dissolved(10min,37kHz),and volume to 50.0ml.The chemical drugs were separated on an Agilent Eclipse Plus C18 chromatographic column(2.1mm×100mm,1.8?m)with acetonitrile and aqueous solution of 10mmol/L ammonium acetate(adjust to pH 4.0 with formic acid)as mobile phase under gradient elution at a flow rate of 0.2mL/min.The 29 illegally added in slimming health food were conducted qualitatively and quantitatively analysis by tandem mass spectrometry under multiple reaction monitoring mode(MRM),with product ion scanning(PI)for positive confirmation.The linear correlation coefficients(R2)of 29 chamical durgs in the three kinds of matrix(slimming tea,capsules,tablets)were more than 0.99,and the precision expressed as relative standard deviations(RSDs)were less than 8.0%.The relative standard deviations(RSDs)of 29 chamical durgs within 24 hours is less than 10%.The recoveries of 29 chemical drugs illegally added in slimming health food at different spiked concentrations ranged from 67.5% ~114.9%.The limits of detection(LODs)were in the range of 0.3~250.7ng/g.This method is rapid,accurate and sensitive with a high degree of separation,and can be used for the simultaneous detection of the 29 illegally added chemicals in slimming health foods.In this subject,high-performance liquid chromatography-high-resolution mass spectrometry(HPLC-LTQ-Orbitrap MS)was used to establish the number of the 29 illegally added chemicals in slimming health foods.Using a data dependency scan,The database was created based on the primary and secondary mass spectra.The quality of the method is high(the mass error of LTQ-Orbitrap MS can be controlled within 5ppm).The precise molecular weight of the compound can be obtained according to the first-order mass spectrum,and the molecular structure of the compound is determined by the second-order mass spectrum.It is also can detect the29 illegally added chemicals in slimming health foods in the absence of reference substances. |
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