Determination Of 38 Kinds Of Illegally Added Drugs In Diet,Lipid-lowering And Laxative Health Food By UPLC-MS/MS

With the booming development of health food industry in recent years,the quality and safety problems of health foods are frequent,and some illegal merchants are driven by interests to illegally add various drugs to health foods,so as to promote consumers to quickly achieve the expected effect after taking them,so that the illegal acts of seeking profiteering are increasingly rampant.However,in the process of routine supervisory inspection,the detection rate of illegal addition of health foods in supervisory sampling inspection is getting lower and lower.The main reason for this is that the illegal acts of illegal merchants are becoming more and more secret,deliberately avoiding the addition of drugs under strict national control,and instead adding their isomers,compounds,or other categories of drugs with similar functions.The purpose of this topic is to establish a detection method with simple and rapid pretreatment,stable and reliable quantitative analysis ability and higher resolution as well as lower detection limit,expand the detection coverage on the basis of national supervision and control items,increase the drugs with similar function claims,select multiple drugs that are easy to be illegally cross-added as the detection objects at the same time,and realize the one-time high-throughput screening of diet lipid-lowering laxative health foods.The research content of this subject is divided into six parts:Part ?: Selection of extraction systemIn order to obtain sufficient extraction of 38 compounds simultaneously from diverse health food matrices,a total of four extraction systems,acetonitrile,methanol,water,and ethanol,were investigated in this study.Finally,methanol was selected to extract the target substance in the sample,and then 10% methanol in water was used for further dilution.It can make the extraction efficiency of the target,reduce the difficulty of purification filtration,effectively avoid the solvent effect in the detection,obtain excellent detection peak shape and resolution,and meet the experimental needs.Part ?: Optimization of separation systemIn order to simplify the detection method and screen 38 compounds simultaneously,the selection of separation system is very important.In this study,the mobile phase system,gradient elution program,and column were selected and optimized.After comprehensive consideration,acetonitrile-0.1% formic acid aqueous solution was selected as the mobile phase system of this method,and the gradient elution program with better mobile phase starting ratio,proportional shift time,maximum organic phase concentration ratio,and proportional change curve was determined,and the chromatographic column with better separation effect was selected comparatively.The effective separation of 38 compounds was achieved,and all 38 compounds could obtain better peak shape and higher resolution,which is of great significance for the reduction of detection limit and the improvement of detection sensitivity in this study.In particular,methamphetamine and triptolamine,phenylpropanolamine and norpseudoephedrine,pseudoephedrine and ephedrine isomers were effectively separated,which played a key role in the accurate characterization of the compound.Part ?: Optimization of Mass Spectrometry and Establishment of Segmented Acquisition MethodMass spectrometry has high sensitivity and resolution,and has great advantages in qualitative and quantitative aspects.In order to achieve the maximum response of each compound and improve the detection sensitivity of experimental methods,all relevant mass spectrometry parameters were optimized in this study.In this study,electrospray ionization(ESI)source,positive ion scanning mode,according to the peak time of each compound,reasonable segmented acquisition,detection.After a series of optimization,the mass spectrometry detection can play the optimal detection efficiency,obtain the maximum compound response value,effectively improve the detection sensitivity and reduce the lower limit of detection of compounds,so that the illegal addition of health foods can be more effectively detected and the missed detection due to insufficient sensitivity can be avoided.In particular,the reasonable segmented acquisition of compounds effectively improves dwell time during the detection of each compound and increases the scanning accuracy.This is decisive for this test method to reduce the detection limit and improve the sensitivity.Part ? Methodological validationIn this study,the linear range of the standard curve was explored,and the detection limit,spike recovery experiment and precision study were carried out.The results showed that 38 target substances had good linear relationship within the concentration range of 5 ? 100 ng/m L,the correlation coefficients were all greater than 0.995,the detection limits were lower than 0.2 mg/kg,the average recoveries of target substances were between 70.8% ? 107.2%,and the precision range was 2.1% ?5.9%,which confirmed that the method was operable and the detection results were stable and reliable.Part ?: Sampling inspection and testing of samples under entrusted inspection at national and provincial levels in 2019 and 2020A total of 146 batches of health foods claimed to have weight loss,lipid-lowering or laxative,including capsules,pills,tablets and liquid preparations,with the detection rate of 38 target compounds of 28%,were inspected by the method established in this study in 2019 and 2020,confirming that the detection method established in this study can be used as a reference for routine illegal addition and inspection of health foods and is feasible.The feasibility of the method was verified through national sampling inspection,provincial sampling inspection and entrusted inspection of health foods in 2019 and 2020.