A Methodology To Quantify EDCs And PPCPs In Wastewater By GC/MS And UPLC/MS/MS

In recent years, many researches have found that some trace contaminats like EDCs and PPCPs in the concentration ofμg/L or ng/L, which are found commonly in water environment, will have negative impact on origannisim. In order to establish a set of methods to collecte, purify, concentrate and analysis the EDCs and PPCPs in the wastewater sample, Estrone(E1), Estradiol(E2), Ethinyl Estradiol(EE2) and Galaxolide(HHCB), Tonalide(AHTN), Ciprofloxacin(CIP), Trimethoprim(TMP) were slected as the representatativees of the EDCs and PPCPs, respectively. Moreover, the removal rates of different treatment units in various wastewater treatment technologies were investigated. The main results and conclusions are show as follows:(1) GC/MS is suitable to analysis HHCB and AHTN.The column temperature program was as follows:run at 100℃and held for 1.5 min, then increase the temperature to 140℃with a rate of 20℃/min and held for 7 min, continue to increase temperature to 180℃with a rate of 2℃/min to 180℃, eventually temperature was increased to 300℃with a rate of 20℃/min and kept for 5 min..The injector temperature was set at 250℃with manual injection (1μL), which was performed in splitless mode by adopting Helium as the carrier gas with speed of 1 mL/min.The mass conditions:The capillary column was coupled directly to the ion source which was operated in active electron impact (EI+) ionization mode. Emission current was 170μA, The ion source temperature was kept at 200℃, and MS transfer line temperature was kept at 250℃. The quantition ion of HHCB was 258.4>213 with retention time of 25.21min. Meanwhile, the quantition ion of AHTN was 258.4>187 with retention time of 25.70 min.The quantitative curves of HHCB was Y=10750X+68530 with linear range of 1μg/L-500μg/L, R2=0.9984. AHTN was Y=7809.5X+21738 with linear range of 1 μg/L-500μg/L, R2=0.9988. The MDL (method detect limite) of lng/L were reached by both curves.(2) EDCs (E1, E2, EE2) and partical PPCPs (CIP, TMP) are suitable to be assessed by UPLC/MS/MS analysis.The mobile phase of EDCs were water and acetonitrele, while PPCPs are water with 0.01% formic acid (FA) and acetonitrile with 0.01% FA were used as mobile phase of PPCPs. the substances were quantified by ussing external standard with optimization mobile phase and mass method. The linear range of 5 EDCs and PPCPs respectively from 0.1 ng/L,0.25 ng/L,0.5 ng/L to 500 ng/L. linear relative coefficient R2 were higher than 0.995. In addition, MDL of 5 substances ranged from 0.05 ng/L to 0.2 ng/L.(3) High efficient of purifiing and extracting of EDCs and PPCPs from wastewater sample were guaranted by using the SPE as the core process and centrifugation, filtration and other process as pretreatment. The recoveries of pretreatment method were between 76.07 and 102%. Relative standard deviations (RSD) were less than 4.37%.(4) The daily operation of UPLC/MS/MS was given. All the possible reasons that may induce the pollution of the UPLC/MS/MS and the correspanding solutions were presented too.(5) The investigation results on the remove of EDCs and PPCPs in sewage treatment plants (STPs) showed that the remove mechanism of estrogens and polycyclic musks are mainly realized by adsorption because of the high Kow. E1 effluent from traditional active sludge plants are higher than that of E2, which may be indued by the transferation fromE1 to E2. Moreover, the remove mechanism of CIP in STPs nay be the biodegradability of bacterics in active sludge. TMP remove efficiency is not distinctness.