Studies And Applications On Microwave Assisted Headspace Solid-Phase Microextraction

Microwave assisted Headspace Solid-Phase Microextraction(MA-HS-SPME)is a novel sample pretreatment technique,which combining the high efficient of microwave extraction and the high enrichment of SPME.It has a high sensitivity,recovery and stability.In this study dynamic microwave-assisted headspace solid phase microextraction was established to improve the enrichment ratio.Then dynamic microwave-assisted headspace solid phase microextraction(DMA-HS-SPME)were used to qualitative and quantitative.And also dynamic microwave-assisted headspace solid phase microextraction and static microwave-assisted headspace solid phase microextraction were compared.A brief description was given as follows:1.An overview about the development process,theoretical basis,factors affecting the extraction efficiency and the application of DMA-HS-SPME was summarized,as well as a detail review of the research of the volatile components of celery and garden chrysanthemum,polycyclic aromatic hydrocarbons,Benzophenone-type UV Filters.2.With celery and garden chrysanthemum as the research object,the volatile constituents of them were successfully extracted by dynamic microwave-assisted headspace solid phase microextraction(DMA-HS-SPME)coupled with four modes of sample treatments and identified by GC-MS.Compound species identified by DMA-HS-SPME method was more than the other three methods,and was helpful to the extraction of semi volatile substances.The results showed that these methods were all simple and feasible for plants volatile constituents analysis.3.A novel method for the determination of 10 polycyclic aromatic hydrocarbons(PAHs)in water samples by gas chromatography-mass spectrometry with dynamic microwave assisted headspace solid-phase microextraction was proposed.Compared with static microwave assisted headspace solid-phase microextraction,it has higher sensitivity.Factors affecting the extraction efficiency such as the power,time of Microwave and the effect of salts were investigated in detail.640 W,15 min and saturated salt water were selected as the optimalizing conditions.The proposed method provided a good linearity(r=0.996?0.999).The limits of detection(S/N=3)were in the range of 0.002?0.037 ?g/L.The relative standard deviations(RSDs)for the determination of 5 ?g/L PAHs were in the range of 2.77%?8.05%(n=5).The results showed that these methods were all simple,fast,easy to operate,without purification steps,less consumption of reagent for the determination of polycyclic aromatic hydrocarbons in water.4.An analytical method for the determination of 3 kinds of benzophenone-type UV filters in packing material of food has been developed by using gas chromatography coupled with tandem mass spectrometry followed by microwave-assisted headspace solid-phase microextraction.The time and power of microwave had been optimized.The calibration curves of the 3 UV filters were linear in the range of 0.0127-0.381 mg/dm2,with a correlation coefficient(r)of 0.991-0.994,the limit of detection(S/N?3)of 0.1137?1.4468 ?g/dm2,and the quantitation limits(S/N?10)were 0.3791-4.8228 ?g/dm2.The average recoveries were in the range of 68.1%?115.6%for the 3 analytes with RSD(n=6)of 4.32%?5.37%.Combining the high efficient of microwave extraction and the high enrichment of SPME,this method was quick and easy,without purification steps,consumption less samples,high efficiency and no pollution.So this work proposes a new method to analyze Benzophenone-type UV Filters in packaging material of food.