| The phenomenon of illegal addition and use of drugs is widespread,posing a huge threat to human health.Regarding the detection of illegal addition and use in food,it is very important.However,most of the current detections are post-test,with a certain lag,and most of them are tested products.The testing method is random inspection,which may face unnecessary waste and influx of untested products.The adverse effects caused by the market.Therefore,if prevention is the purpose of testing,such problems will be avoided to a certain extent,and product safety will be ensured to a greater extent.To achieve the purpose of prevention,there is no doubt that the detection window needs to be moved forward,for example,focusing on the production or breeding site,so fast and higher requirements for detection methods are put forward.Among the many rapid detection methods,the detection products are mainly used and are more complicated;and the ion mobility spectrum passes through the collision of the ions entering the electric field with the neutral gas,and migrates according to the mass-to-charge ratio,volume,etc.,to complete the separation,and has a certain degree of resistance.Interference ability,fast detection speed,and certain development potential.Because of its atmospheric pressure ionization source,it is easy to produce complex ions during detection,and illegal addition has problems of drug metabolism,low content,and complex sample matrix.Therefore,it is necessary to adapt to fast and efficient sample purification.To this end,this article uses ion mobility spectrometry as a detection method to study a fast sample pretreatment method that matches it to meet the detection purpose of illegal drug addition and use.Part one:Rapid detecting of malachite green and crystal violet illegally added in aquaculture water by polyvinylidene fluoride microporous membrane covered with immobilized grapheme oxide module combined with ion mobility spectrometryObjective:A rapid and efficient method for the purification of trace malachite green(MG)and crystalline violet(CV)from aquaculture water was established by studying the efficient pretreatment method of immobilized GO covered polyvinylidene fluoride microporous film module combined with ion migration spectroscopy.Methods:Graphene oxide(GO)was synthesized by Hummers method and characterized by ultraviolet spectroscopy,Fourier transform infrared spectroscopy and scanning electron microscopy.According to the literature,the polyvinylidene fluoride(PVDF)microporous filter membrane was successively put into the prepared polydopamine-Tris-HCl buffer solution and GO solution for reaction,drying,and then the GO coating filter membrane was obtained.The clean SPE membrane was curled and freely attached to a 10 m L centrifuge tube,then 10 m L sample solution was added for eddy adsorption and the sample solution was discarded.Ultrapure water cleaning film and centrifugal tube;2 m L methanol was added for eddy elution for 10 min,and the eluent was injected into ion mobility spectrometry(IMS)for detection.Results:The recoveries of CV and MG were above 93.3%,and the enrichment ratio was about 35.MG was linear in the range of 5.19-519.5ng/m L,and R~2was 0.99.CV was linear in the range of 5.12-512.5 ng/m L,and R~2was 0.99.LOD was 0.85 ng/m L and 1.09 ng/m L,respectively,and the process was simple and rapid.Conclusions:This study established a simple and rapid breeding of CV and MG in water analysis method,by building GO microporous film plated sample purification methods,and IMS adapter,can quickly complete the whole sample processing and testing process,a single analysis only 18 min,meet the requirements of on-site rapid detection,is expected to provide a means of selection of site supervision.Part two:Determination of amantadine and rimantadine residues in honey by ESI-IMSObjective:A rapid and simple direct extraction-ion mobility spectrometry method was developed for the rapid detection of amantadine(ATD)and rimantadine(RTD)residues in honey matrix.Methods:1 g honey sample was placed in a 50 ml centrifuge tube,extracted with 5 ml of 1%formic acid cyclohexane by ultrasonic,centrifuged at 8000 R/min for 5 min,and then the supernatant was blown with nitrogen.0.5 ml methanol was used to dissolve and mix well for ion mobility spectrometry analysis.Results:The linear range of ATD was 0.010-10.1μg/ml,and that of RTD was 0.010-10.4μg/ml.the detection limits were 0.40 ng/ml and 0.50 ng/ml,respectively.There was no matrix interference in the analysis of honey samples,and the recovery was not less than 91.4%.Conclusions:The established method can be used to determine the ATD and RTD in honey simply and quickly,and the operation is simple.The honey sample can be processed in a few minutes.Combined with ESI-IMS detection,the single analysis only takes 16 minutes.Therefore,this study provides a new method for the rapid detection of drugs in honey.Part three:Rapid determination of amantadine in saliva by ion mobility spectrometryObjective:The simple liquid-liquid extraction method was used for rapid treatment of ATD in saliva samples and IMS analysis,which was intended to provide a rapid and effective means for ATD concentration monitoring in biological substrates.Methods:The 50 L saliva sample was taken,Na OH(2 M,200μL)was added to make the sample alkaline,3 m L of freshly distilled extractant n-hexane was added,and the sample was vortex mixed for 5 min.The n-hexane layer was centrifuged for 5 min at 4000 r/min at room temperature.The n-hexane layer was blown dry with nitrogen,and 200μL methanol was redissolved,then the sample was injected into IMS for rapid analysis.Results:The linear range of ATD was 0.300-5.00μg/ml;the detection limit of the method was 0.077μg/ml;the recovery of ATD was 91%-105%,and there was no matrix interference in the analysis of saliva samples.The whole process was simple and rapid.Conclusions:The established rapid detection method of amantadine in human saliva is simple and fast,and can be completed within 12 minutes,which provides a new rapid analysis method for drug driving detection. |
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