| Environmental hormones which could interfere with the normal function of the human endocrine system regulation, and lead to abnormal effects, have caused harm to the organism growth. So environmental hormones that widely existed in natural environment had aroused people’s great attention. Environmental hormones have the characteristics of lipophilic which can easily enriched in the sewage sludge, while the sludge matrix composition is very complicated that brought great disturbance and difficulties to analysis the environmental hormones in it. Therefore, researching on the problem between pretreatment methods and its monitoring analysis has great significance.Matrix Solid Phase Dispersion (MSPD) extraction has the characteristics of using less consumption of samples and organic solvents and allowing high extraction efficiency, which the equipment is cheaply and easily available, and the operating rapidly and simply. The MSPD extraction is worth studying in sewage sludge samples to extracted environmental hormones.The main content of study includes the following parts:1. Generally introduced the common environmental hormones, several commonly pretreatment technology and their advantages and disadvantages which used in the sewage sludge samples, then expounded on DMPD, including its principle, operation steps, influence factors, and application situation in the last.2. A matrix solid-phase dispersion (MSPD) extraction with high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was established for the simultaneous determination of3phthalic acid esters (PAEs) in sewage sludge. Several important influence factors about the extraction efficiency were optimized, including the selection and the amount of extraction solvent, grinding time, the selection and amount of eluent, choice of cleaning agent, etc. Under the optimal conditions3kinds of PAEs have good linear relationships in the concentration of2-100ng/g, with the correlation coefficients are between0.9973to0.9981. And the limits of detection (LODs) ranging from0.012to0.056ng/g, the relative standard deviations (RSDs, n=3) for Actual sewage sludge samples were between1.7%and7.3%, the recoveries of actual samples can reach86.2%to103.4%. As a result, it was feasible to simultaneously determinate phthalic acid esters in sewage sludge.3. Followed with further validation, matrix solid-phase dispersion extraction technology coupled with HPLC-MS/MS was applied to determination of six estrogens (estriol, estradiol,17a-ethinylestradiol, estrone, diethylstilbestrol and bisphenol A) in sewage sludge. The optimum experimental conditions were determined:The0.3g sewage sludge sample was mixed with the1.5g Florisil to homogeneous for15min by shocking abrasive in grinding balls, then transferred the mixed sample to a column and eluted by the6mL methanol. Using the HC-C18as cleaning agent to purified the eluent and concentrate the supernatant to0.6mL by nitrogen, then analyzed qualitatively and quantitatively by UPLC-MS/MS in the last. The6target estrogens can achieve the good linearities in the ranged of1-50ng/g, with correlation coefficients above0.992. And the limits of detection (LODs) for target compounds were ranging from0.12to0.25ng/g. Average recoveries of6analytes at three spiked levels ranged from81.4%to107.3%with relative standard deviations (RSDs) of1.8%-9.7%. The method was rapid, sensitive and reliable, and suitable for the simultaneous determination of trace estrogen in sewage sludge.4. Finally, summarized the two parts of experimental section. Matrix solid-phase dispersion extraction does not require expensive equipment and strict experimental conditions, also have shortly extraction time and high extraction efficiency, that could be used to extracting sewage sludge samples. Thereby, matrix solid-phase dispersion extraction could expand the range of applications in sewage sludge, and have considerable development prospect. |
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