Study On Simultaneous Detection Of Varied Illegally Added Illegally In Tea Products By Liquid Quality Method

Based on the investigation and analysis of risk monitoring of health food tea products in Zhejiang Province,this study aimed at the social phenomena and potential risk problems of tea products which claimed to have anti-rheumatism and hypoglycemic effects,and detected the possible illegal addition of anti-rheumatism drugs and auxiliary hypoglycemic drugs in tea products.Through the screening of pretreatment method and purification technology,combined with UPLC-MS/MS method optimization,a fast and efficient method for simultaneous detection of multiple illegally added drugs was established.This content can be directly used for the detection and safety evaluation of many kinds of illegally added drugs in tea products,aiming to provide support for the formulation of standards and technical testing of illegally added drugs.The main research contents and results are as follows:1.Through the investigation of supervision,sampling and risk monitoring of health food and tea products in Zhejiang Province in recent three years,it was found that the problem of illegally adding chemical drugs in tea products was more serious,and then the reasons for the problems were analyzed and a series of supervision suggestions were put forward.The unqualified rate of auxiliary hypoglycemia in tea products is higher than that in other categories.At the same time,the anti-rheumatism detection technology in tea products is relatively weak.It is necessary to establish a sensitive,reliable and rapid detection method for adding many illegal drugs in tea products.2.By normalizing the methods of supplementary inspection and approval documents of national food and drug inspection,the qualitative technology is improved to the quantitative technology.A method based on UPLC-MS/MS was developed for the rapid detection of 13 anti-rheumatic drugs illegally added in tea products.Specifically as follows: After ultrasonic extraction by methanol,the samples were eluted by 0.1% formic acid solution-acetonitrile as mobile phase gradient,separated by chromatographic column,ionized under ESI source positive ion mode,and analyzed qualitatively and quantitatively by multi-reaction monitoring mode.Results showed that the limits of detection(LOD)for 13 anti-rheumatic were in the range of 0.3-1.6 ?g/kg and the limits of quantification(LOQ)were in the range of 1.4-6.5 ?g/kg.The average recoveries at three spiked levels ranged from 80.2% to 110.3%,with relative standard deviations(N=6)of 2.1%~9.6%.3.By means of pretreatment,selection of extraction solvent,optimization of liquid chromatography and mass spectrometry.A method was developed for the rapid detection of 11 kinds of illegal added supplementary hypoglycemic agents in tea products.The samples were extracted with methanol by ultrasonication,After chromatographic separation on column with 0.1% formic acid solution-methanol as mobile phase,the target compounds were qualitatively and quantitatively determined under the multiple reaction monitoring(MRM)mode in positive ionization mode.Results showed that the linear relationship of 11 kinds of auxiliary hypoglycemia was good,and the correlation coefficient was above 0.9987.The limits of detection(LOD)were in the range of 0.001~0.545 mg/kg and the limits of quantification(LOQ)were in the range of 0.004~1.797 mg/kg.The average recoveries at three spiked levels ranged from 83.73%~109.97%,with relative standard deviations(N=6)of 2.2%~6.8%.