Simultaneous Determination Of 45 Chemical Drugs Illegally Added In Auxiliary Antihyperglycemic,Antihypertensive And Antihyperlipidemic Health Foods By High Performance Liquid Chromatography-tandem Mass Spectrometry

At present,the official detection methods post by the State Foods and Drug Administration including 28 kinds of antihypertensive,antihyperglycemic and antihyperlipidemic drugs,which can no longer meet actual regulatory needs.Therefore,according to the efficacy of the chemical drugs,it is vital for us to develop a large capacity detection method,which can detect multiple illegally added chemical drugs in auxiliary antihyperglycemic,antihypertensive and antihyperlipidemic health foods simultaneously.In the study,a method for the simultaneous detection of 45 chemical drugs illegallyaddedinauxiliaryantihyperglycemic,antihypertensiveand antihyperlipidemic health foods by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed.The samples(including tea,soft capsules,hard capsules,tablets)used 90%aqueous methanol ultrasonic extraction(10min,37kHz),and made up to 20 mL by 90%aqueous methanol after cooling,then diluted by 20%aqueous acetonitrile.The chemical drugs were separated on an Agilent Eclipse Plus C18 chromatographic column(2.1 mm×100 mm,1.8μm)with acetonitrile and aqueous solution of 5 mmol/L ammonium acetate(adjust to pH 3.0with formic acid)as mobile phase under gradient elution at a flow rate of 0.2mL/min.The 45 chemical drugs illegally added in auxiliary antihyperglycemic,antihypertensive and antihyperlipidemic health foods analyzed under multiple reaction monitoring mode(MRM),while product ion scanning(PI)was used for positive confirmation.The linear correlation coefficients(R~2)of 45 chemical drugs were more than 0.99,and the precision expressed as relative standard deviations(RSDs)were less than 9.7%.The relative standard deviations(RSDs)of 45 chemical drugs within 24 hours were less than 9.9%.The recoveries of 45 chemical drugs at different spiked concentrations ranged from 63.3%~129.5%.The limits of detection(LODs)were in the range of 0.02~128 mg/kg.The method has simple pretreatment,short analysis time,good sensitivity,high specificity,good accuracy,and is applicable to be used for the simultaneous detection 45 chemical drugs illegally added in auxiliary antihyperglycemic,antihypertensive and antihyperlipidemic health foods.In the study,high-performance liquid chromatography-high resolution mass spectrometry(HPLC-LTQ-Orbitrap MS)was used to establish a database of the 45chemical drugs illegally added in auxiliary antihyperglycemic,antihypertensive and antihyperlipidemic health foods.The database was created based on the retention time,accurate mass of parent ion and product ion and isotope peak through full MS/dd-MS~2mode.By this database,it is possible to detect 45 chemical drugs illegally added in auxiliary antihyperglycemic,antihypertensive and antihyperlipidemic health foods in the absence of reference substances.