Study On High Throughput Screening Method Of Prohibited Drugs In Health Foods

With the increasing demand for health food,the market of health food is expanding,and the market competition is becoming increasingly fierce.It is common for manufacturers to illegally add prohibited drugs in order to obtain curative effect.However,the national food safety supervision rules specify a single type of health food testing methods and complicated operation.Because of the inadequate precision,it is not in conformity with the requirements of market supervision.A high-throughput,high-efficiency and accurate detection method is urgently needed to ensure the market safety of health food.1.According to the National Food Safety Supervision and Sample Inspection Rules,a pretreatment method for detecting 68 kinds of illegal additives in health food was established.After grinding and other pretreatment of health food,1%formic acid-methanol solution was added for ultrasonic extraction for 20 minutes,and the volume was fixed to 50 mL.The method was purified by QuEChERS dispersive solid phase extraction kit.The method was simple,effective in reducing matrix interference and enhancing the detection accuracy.2.A high performance liquid chromatography-triple quadruple ion well mass spectrometry(HPLC-QTRAP-MS)method was developed for the simultaneous determination of 68 illegal additives in health food.Acetonitrile and l0mmol/L ammonium acetate solution were used as mobile phase for gradient elution at 250 L/min flow rate,separated by phenomenex Kinetex C18 column(50mm 2.1mm,2.6?m),analyzed by compound scanning mode(MRM-IDA-EPI),confirmed by enhanced secondary fragment(EPI)database and quantified by external standard method.The correlation coefficient R2>0.999,the minimum detection limit is 0.01 ng/g?1.05ng/g,the precision(RSD)is less than 6%,the recovery rate is 84.1%?105.9%.Good stability in 24h,and the relative standard deviation is less than 5%.The method has high flux and high sensitivity,and is suitable for the determination of 68 prohibited drugs in health food.3.In this research,68 kinds of drug-enhanced composite secondary fragment ion(EPI)atlas databases were established by using high performance liquid chromatography-QTRAP-MS.According to the unique EPI mass spectra of each compound at different energies(high,medium and low),a "fingerprint" pattern is formed,which can effectively eliminate false positives.It realizes the search and confirmation without standard products,overcomes the drawbacks of traditional mass spectrometry analysis,and enhances the accuracy of detection and analysis.This method achieves qualitative,quantitative and confirmatory verification at the same time.It is characterized by simple operation,large flux,high sensitivity and high accuracy.It provides technical support and scientific basis for the quality control and safety evaluation of health food.