Screening of Non Target Compounds in Wastewater Samples

Screening of Non Target Compounds in Waste water SamplesReportSince October 2012, I have worked in a special project ab aside exclusion of pharmaceuticals and organic mixeds Development of concepts and novel, cheap cleaning procedures Formation of metabolites by ozonoation. It was a kind of training for me and a special key for my PhD work. We argon fire in screening of non target compounds in wastewater samples. Wastewater samples argon collected from distinct wastewater discussion plants at polar divvy upment points. For example before ozonation, subsequently ozonation and after biological handling steps. These compounds are picked by material phase extraction (SPE) system development trustworthy solid material ( harbor HLB). This kind of SPE is suitable to extract hydrophilic and lipotropic analytes. We did several steps to extract those compounds using dissimilar procedures and different analyzing tools. We utilise HPLC-UV, LC-MS and GC-MS to fail the extracted compounds. The toxicological tests are achieved for each sample in site to discover the efficiency of wastewater treatment and the effect of treatment to see new unknown transformation products.In this project, I learned so more things likeHow to validate and develop a manner to extract polar and non polar compounds from wastewater matrixes using certain SPE steps.How to choose the topper solid phase materials to extract a wide range mutual opposition of chemical compounds in wastewater matrixes.Getting the principles for handling of different analytical instruments to validate specific rules and to analyze the extracted compounds.Taking enough time to look backward the statistical principles which are necessary to find the optimum ways for treatment.Achieving the possibilities to analyze the output info and comparing different procedures to find out the lift out angiotensin converting enzyme for analysis.Combining chemistry with biology in order to prise the toxicologica l estimates and to know the best wastewater treatment step. directly, I am working on developing a method to extract the chase six compounds from water matrixCatechol, trans,trans-Muconic acid, p-Benzoquinone, 1H-Benzotriazole, p-Nitrophenol and 2,6-Dichloraniline.Catechol, trans,trans-Muconic acid and p-Benzoquinone are transformation products generated after treatment of the parent compound (Bisphenol A) with ozone in aqueous solution (water). Bisphenol A (BPA) belongs to the numerous anthropogenic compounds considered as endocrine disruptors. Although less estrogenic toward aquatic organisms than natural hormones, BPA has been describe to be able to induce feminization phenomena in various species of animals. BPA is commonly apply for the production of polycarbonate plastics and epoxy resins. It is also used as stabilizer or antioxidant for many types of plastics much(prenominal) as polyvinyl chloride (PVC). BPA is observe with a high frequency in surface waters.1H-Benzotria zole has been found in wastewater and the subsequently impacted surface water. This compound is employed to interdict metal corrosion and as UV-inhibitors, and found to use in applications such as airplane deicing fluids, dishwashing detergents, and plastic formulations.p-Nitrophenol is degradation product generated end-to-end the ozonation process of the antibiotic sulfamethoxazole. Sulfamethoxazole in combination with trimethoprim is used to treat a wide range of human diseases, such as urinary and respiratory tract infections. thither are many publications that have reported about the presence of this antibiotic do drugs in sewage treatment plants, hospital effluents and rivers. Besides, this compound might be expected to be defend in groundwater, because the antibiotic sulfamethoxazole is also applied to animals as product promoter.2,6-Dichloraniline is a metabolite produced after ozonational step of the drug diclofenac in aqueous solution. Diclofenac is one of the most comm only used pain killers. It is used to treat wicked conditions such as arthritis, sprains and strains, gout, migraine, dental pain, and pain after surgical operations. There are many articles that have reported about the presence of this drug in sewage treatment plants.First step, I inclined(p) different standard solutions for each compound, then validated and developed a method to analyze these compounds by using HPLC-UV instrument. A mixture of methanol and water (pH=2) are used at certain progress time and different ratios to obtain the best LC chromatogram with good separation and resolution for each compound in the mixture. The maximum wavelength () for each compound is known by using UV-spectrophotometer. add-in (1) summarizes the information obtained after analyzing my target compounds by HPLC-UV.Table 1 plaza Retention time tR (min) (nm)Catechol (1)26.35278t,t-Muconic acid (2)28.43278p-Benzoquinone (3)30.462781H-Benzotriazole (4)34.42278p-Nitrophenol (5)39.892282,6-Dichlor aniline (6)48.04228Figure (1) shows the HPLC-UV chromatogram (relative response in mV vs. tR) for a mixture of six compounds in one ready stock solution.5 6Figure 1 2 4 1 3In order to develop a method to analyze the target compounds the limit of detection (LOD) and limit of quantification (LOQ) should be mensurable in order to know the sensitivity of HPLC-UV instrument towards each compound.The LOD look upon for each compound was calculated from a chromatogram on the basis of signal/noise (S/N) ratio of 3.The LOQ value for each compound was calculated from a chromatogram on the basis of signal-to-noise (S/N) ratio of 10.Table (2) shows the values of LOD and LOQ for each compound.Table 2Substance LOD(ng/L) LOQ(ng/L)Catechol (1)8.829.3t,t-Muconic acid (2)1.24.0p-Benzoquinone (3)6.321.01H-Benzotriazole (4)8.528.3p-Nitrophenol (5)27.491.32,6-Dichloraniline (6)18.060.0For linearity and statistical evaluation, I prepared mixture solutions of six compounds at concentrations of 0.1, 0. 25, 0.4, 0.55, 0.7, 0.85 and 1.0 mg/L.Table (3) shows the statistical data for the prepared stock solution of 0.7 mg/L.Table 3Substance % Relative response Correlation coefficient (r)Catechol (1) atomic number 60.999t,t-Muconic acid (2)1010.999p-Benzoquinone (3)1060.9991H-Benzotriazole (4)1000.999p-Nitrophenol (5)1000.9992,6-Dichloraniline (6)1040.999The linearity at my working range is shown as followsNow I am working in developing a readying method to extract these compounds from water matrix by using different solid phase materials. Up to now, I tried two types of solid phase cartridges OASIS HLB and SPEED DISK cartridges. Its noticed that OASIS HLB gave higher recovery than SPEED DISK.In order to find out the best solid phase material, I go out try many types of SPE.After finishing this step, I will develop a method to extract and analyze about 30 chosen chemical compounds which are produced after the ozonation process of pharmaceutical and parent compounds in water matrix. Th ese compounds will beDiclofenac, 2,6-Dichloroaniline, Metoprolol, Sulfamethoxazole, 4-nitrophenol, Bisphenol A, Catechol, trans,trans-Muconic acid, cis,cis-Muconic acid, p-Benzoquinone, Ciprofloxacin, Paracetamol, 1,2,4-Benzenetriol, Oxalic acid, Succinic acid, Malic acid, Malonic acid, Oxaloacetic acid, Hydroquinone, Maleic acid, EDTA, Glyoxylic acid, Formaldehyde, Carbamazepine, Glyoxylic acid, Oxamic acid and 1H-Benzotriazole.