Research Of Nitrogen Impurity Calixarene Stationary Phase On The Enrichment Of Trace Pollutants In The Environmental Water

Rapid separation and accurate determination of trace concentrations of component in complex system is an important and difficult task that today’s analytical chemists are faced with. As the sample matrix becomes more and more complex, the content of analyte becomes lower and lower, the development of high efficiency, the preparation of simple and green samples and the pretreatment technology have been an important research subject. SPE (Solid-Phase Extraction, SPE) is a mainstream sample pretreatment technique developed in recent years which is combined with liquid-solid Extraction and column liquid chromatography.SPE is based on the analytes’different allocation or intereaction in the solution and the SPE materials to achieve the target of analytes’ retention.After the eluent eluting the analytes,we can achieve the purpose of separation, purification and enrichment.Calixarene is the third generation of macrocyclic molecules after cyclodextrins and crown ether. In the body of the novel compounds that mixed aromatics is treated as the bridge of heteroatomic cup, impurity nitrogen or oxygen atom replaces the methylene bridge of the traditional calixarenes. After aromatic heterocyclics (such as pyridine, triazine, etc.) replacing phenol groups of calixarene,the nitrogen atom, as a connecting bridge, can use sp2, sp3, or a variety of hybrid states between the two, and can form conjugated effect of different levels with adjacent aromatic heterocyclics. The introduction of the impurity atoms and aromatic heterocyclics makes the host moleculars possess rich diversities in the respect of conformation, molecular recognition performance. Compared with ODS, Cup (miscellaneous) aromatics chromatography stationary phase, has cooperative interaction,π-π interaction, π-electron transfer and hydrogen bonding, electrostatic effect, etc besides hydrophobic effect. This paper systematically studies the new four nitrogen impurity calix [2] arene [2] triazine bonded silica gel stationary phase (NCS) extracts and concentrates the trace pollutants in the environmental water as solid-phase extraction material. This thesis is mainly divided into the following three parts.Firstly, as solid-phase extraction material, NCS enriches2-nitrotoluene,2,4-dinitrotoluene and TNT in the environmental water. Setting up the replication of NCS-SPE-HPLC to detect three kinds of nitrobenzene class material in actual samples. Three kinds of material had good linear range in0.5-50ng/mL(R2>0.993),the detection limit is in0.1-0.3ng/mL, quantitative limit is in0.3-1.0ng/mL. The recovery ranges of standard addition for tap water and The Yellow River sample were79.96%-91.58%and80.85%-89.77%respectively, the relative standard deviation (RSD) of this method is6.3%or less. This method was high sensitivity, good selectivity and faster.Secondly, establishing a new type of replication NCS-SPE-HPLC to test p-nitrophenol,2,4-dinitrophenol,2,4,6-trinitrophenol in actual water samples.Three kinds of material has good linear in the concentration range of0.5-50ng/mL (R2≥0.993), detection limit was in0.03-0.3ng/mL, quantitative limit was in0.1-1.0ng/mL. The recovery ranges of standard addition for Yellow River and Jin Shuihe sample were75.71%-90.89%and77.42%-93.62%, with the relative standard deviation (RSD) of this method was6.3%or less.The sensitivity、accuracy and precision of such method were satisfactory.Thirdly, establishing a new type of replication NCS-SPE-HPLC techniques to detect environmental hormones contamination diethylstilbestrol. Diethylstilbestrol has good linear range in0.1-50ng/mL (R2≥0.993), the detection limits was0.03ng/mL, quantitative limits was0.1ng/mL. The actual sample of West lake’s standard addition recovery was91.89%-102.4%, relative standard deviation RSD≤5.2%. This method was high sensitivity, good selectivity and faster.