Nutrient dataset development via FAO/INFOODS approach for infant nutritional survey in rural Matiari, Pakistan.

To accurately evaluate dietary intake, multiple resources are necessary, including serving-size modules, pictures, and questionnaires that are used to gather information during surveys. One critical component is the accessibility of food composition data at the national or regional level, which is required to determine dietary intake. Food Agriculture Organization/International Network of Food Data Systems (FAO/INFOODs) tools are useful for developing high-quality food composition data. We used these tools to create a nutrient dataset for a nutritional survey in Matiari, Sindh, and to collect dietary information through a 24-hour food recall questionnaire. The survey results indicated 540 distinct types of foods, including 291 ready-to-eat items, 84 foods used as ingredients in recipes, and 164 various composite and mixed recipes. Most food items corresponded to the national and regional Food Composition Tables (FCTs) and the Food and Nutrient Database for Dietary Studies (FNDDS) of the USDA, with the exception of recipe food data. We utilized Eurofir-recipe calculation methods to compute the recipe data. The data were homogenized and standardized utilizing EFSA and Langual™. Because of the obsolescence and inadequacy of Pakistan's food composition table in assessing essential nutrients, we had to source data from various other sources. Consequently, to establish the nutrient dataset, we incorporated approximately 25 % of user data from national sources, with recipe data comprising 46 % and less than 20 % extracted from regional, U.S database, and diverse online sources. This study is the first effort in which we gathered data from reliable sources representing local eating patterns, with some exceptions. Future studies will hugely benefit from this database, especially as we face a high prevalence of undernutrition in our part of the world.

Fabrication of 1-octane sulphonic acid modified nanoporous graphene with tuned hydrophilicity for decontamination of industrial wastewater from organic and inorganic contaminants.

This research work is based on the fabrication of a graphene oxide-based composite (GOBC) to remove the maximum number of contaminants from different industrial effluents. The GO was first intercalated with 1-octanesulphonic acid sodium salt and subjected to microwave irradiation to produce GOBC. Fixed-bed column tests and Jar-tests were performed for removal of the most harmful endocrine disrupting compounds (EDCs) such as bisphenol A, bisphenol S, endosulphan, beta-estradiol, dyes (methylene blue and violate) and toxic metal ions such as Pb2+, Li+, Ni2+, Co2+, Cr6+, Zn2+, Cd2+, Hg2+, Cu2+, and As5+via adsorption. The prepared material was thoroughly characterized for its unique functional and structural properties. The results obtained from Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller, scanning electron microscopy, Raman spectroscopy, water contact angle and X-ray diffraction analysis confirmed the successful preparation of GOBC using the proposed intercalation/microwave method. The water contact angle results showed decreased hydrophilicity of GOBC as compared to GO as the contact angle of GOBC (77.75°) was higher than that of GO (53.98°). The effects of main column parameters such as bed height, initial analyte concentration and solution flow rate were investigated. The results revealed that shorter breakthrough time, and high adsorption capacity were obtained at high flow rates of 1 mL min-1, while longer breakthrough time and lower adsorption capacity were obtained at lower flow rates of 0.5 mL min-1. The effect of bed depth on the breakthrough curve of analyte adsorption was a steep breakthrough curve; or a shorter breakthrough time occurring at lower bed height. The adsorption data obeyed the Yoon-Nelson and Thomas models very well. The adsorption capacity for BPA, BPS, endosulphan, beta-estradiol, methylene blue and violate was found to be 307, 305, 260, 290, 230 and 195 mg g-1, respectively. The adsorption capacity of GOBC for toxic metal ions such as Pb2+, Li+, Ni2+, Co2+, Cr6+, Zn2+, Cd2+, Hg2+, Cu2+, and As5+ was found to be 156, 136, 126, 124, 118, 114, 82, 82, 72 and 72 mg g-1, respectively with excellent kinetics. The adsorption data obtained using Jar-tests revealed that GOBC obeys a Langmuir isotherm and a pseudo second order kinetics model. The analysis of industrial wastewater samples showed good removal efficiency of GOBC.

Facile Process for the Development of Antiviral Cotton Fabrics with Nano-Embossed Copper Oxide.

Metallic or metal oxide-based nanoparticles have the potential to inactivate viruses. Among various metals, copper has shown edge over others. One of the rapidly evolving areas is to combine nanoscience for production of self-sanitizing antiviral surfaces. In this study, we designed antiviral-coated fabrics to combat the spread of viruses. Copper oxide nanoparticles were sonochemically synthesized and subsequently deposited using the dip-coat process to modify the surface of fabric. The morphology and structure of uncoated and coated fabrics were examined by scanning electron microscopy, X-ray diffraction, FTIR, and elemental analysis. The findings show that small, agglomerated rugby ball structures made of copper oxide (CuO) nanoparticles (16 ± 1.6 nm, according to the Scherrer equation) develop on the surface of fabric, resulting in nano-embossing and a hydrophobic (contact angle > 140°) surface. The CuO-coated fabric yielded the maximum zone of inhibition for antibacterial activity. The virucidal activity (against human adenovirus-B) of CuO nanoparticle-fabricated fabric against adenovirus shows decreased 99.99% according to the ISO 18184 testing standard. With the dip and dry approach, any textile industry can use the simple coating procedure without having to change its textile operations. This fabric can be widely used in the face mask, clothing, bedding, and aprons, and the coating remains efficient over more than 25 washes.

Modeling of cadmium(II) removal in a fixed bed column utilizing hydrochar-derived activated carbon obtained from discarded mango peels.

Cadmium is found in many underdeveloped countries' aquatic bodies. Therefore, contaminated water should be treated before consumption; henceforth, efficient and customized point-of-use filtration is foreseeable. Traditionally, carbon-based sorbents have been utilized for such treatments, but alternative sources are also being investigated. Hydrochars made from mango peels using a thermal activation process were employed as an adsorbent instead of activated carbon in this investigation. The prepared material was porous with active surface functionalities, and the interaction of cadmium with the surface was possibly ion-exchange in nature. The performance of a material for a candle water filtering system with a 2.5 cm internal diameter and a 30.48 cm column height was determined using the parameters acquired by the Thomas model. The material was found to be highly efficient at 453.5 L/min/Filter water, whereas 31670.6 L/min/Filter can be treated if the break point and exhaustion point are considered, respectively, as the candle replacement time. These findings indicate that activated hydrochar might be a suitable sorbent for removing cadmium ions from contaminated water.

Recent Development in Fluorescent Probes for Copper Ion Detection.

Copper is the third most common heavy metal and an indispensable component of life. Variations of body copper levels, both structural and cellular, are related to a number of disorders; consequently, the pathophysiological importance of copper ions demands the development of sensitivity and selection for detecting these organisms in biological systems. In recent years, the area of fluorescent sensors for detecting copper metal ions has seen revolutionary advances. Consequently, closely related fields have raised awareness of several diseases linked to copper fluctuations. Further developments in this field of analysis could pave the way for new and innovative treatments to combat these diseases. This review reports on recent progress in the advancement of three fields of fluorescent probes; chemodosimeters, near IR fluorescent probes, and ratiometric fluorescent probes. Methods used to develop these fluorescent probes and the mechanisms that govern their reaction to specific analytes and their applications in studying biological systems, are also given.

Selenium Contents in Different Types of Raw and Processed Meat Products, Consumed Among the General Population of Pakistan.

The present study was undertaken to generate a database for selenium (Se) content present in minced and processed meat products abundantly available in the market and to estimate the dietary Se intake in different types of minced/raw and processed meat in Pakistan. The concentration of Se was determined in meat samples of different brands of beef, chicken, and mutton, consumed among the local population of different cities of Pakistan. For pretreatment of the meat samples, microwave-assisted acid digestion procedure (MAD) was developed for the Se analysis in the meat samples of different brands. The validity of the designed method was checked by certified reference samples of BOVM-1 (bovine muscle certified reference material 1). Digested meat samples were analyzed by graphite furnace atomic absorption spectrophotometry. Results showed that among different meat types, average Se concentration of beef was close to those of chicken samples. The mean Se concentration in the meat observed in reducing order was established in mutton (120 µg/kg), beef (91 µg/kg), and chicken (90 µg/kg). These results suggest that mutton and chicken samples have significant differences in their average concentrations. There was no significant difference in the average concentration of beef and chicken (p > 0.05), while there was a significant difference in average concentrations of Se in beef and mutton (p < 0.01) meat samples. Mutton minced meat contains higher Se than different branded processed products. As far as variation in brands was concern among mutton samples, B1-minced mutton meat sample contain higher Se (107 µg/kg) followed by B3-shish kabab (123 µg/kg) and B3-meat balls (129 µg/kg). Among minced and processed chicken products, Se ranged from 83 to 97 µg/kg. Whereas in beef samples, B1-minced meat and B3-chapli kabab contain higher Se, i.e., 99 and 92 µg/kg respectively compared with other beef brands. Taking into account, the average daily intake of meat by Pakistani's, the dietary Se daily intake was 4.184, 9.263, and 6.605 µg per capita for mutton, beef, and chicken, respectively.

Preparation, characterization, and binding profile of imprinted semi-IPN cryogel composite for aluminum.

Human body is greatly exposed to aluminum due to its high abundance in the environment. This nonessential metal is a threat to the patients of chronic renal disorders, as it is easily retained in their plasma and quickly accumulates in different tissues. Thus, there is great need to remove it from the aqueous environment. In this study, Al3+ imprinted semiinterpenetrating polymer network (semi-IPN)-based cryogel composite was prepared and applied for the purification of environmental and drinking water samples from aluminum. Poly (2-hydroxyethyl methacrylate) (pHEMA) discs were produced via cryogenic treatment and imprinted semi-IPN was introduced to the 3-(trimethoxysilyl) propyl acrylatemodified macroporous cryogel discs. The adsorption properties and selectivity of the aluminum (III) imprinted semi-IPN cryogel composite were studied in detail. The imprinted semi-IPN cryogel composite showed good selectivity towards aluminum (III) ions with the imprinting factor (IF) of 76.4 in the presence of competing copper (II), nickle (II), and iron (III) ions. The maximum adsorption capacity of 271 µmol g-1 was obtained for aluminum (III) at pH 7.0 within 10 min using imprinted semi-IPN cryogel composite. The good selectivity and reusability of aluminum (III)-imprinted semi-IPN cryogel composite makes this material an eligible candidate for the purification of drinking water from aluminum (III) leaving important minerals remained in the water.

Correction to: Evaluation of hydrochar efficiency for simultaneous removal of diclofenac and ibuprofen from aqueous system using surface response methodology.

The original publication of this paper contain typographical mistakes.

Evaluation of hydrochar efficiency for simultaneous removal of diclofenac and ibuprofen from aqueous system using surface response methodology.

Pharmaceutically active compounds like diclofenac (DFS), ibuprofen (IBP), and other drugs that persist in the environment are listed as emerging contaminants. These escape from normal wastewater treatment plants and find their way to water streams; therefore, alternate treatment processes are needed. Herein, a sorbent material is reported that is prepared through hydrotermal carbonization from dried fruit powder of Zizipus mauritiana L. (HTC-ZM) and applied for simultaneous removal of DFS and IBP. Carbonized material (HTC-ZM) was found as agglomerates of approximately 1 µm particle size with surface area of 1160 m2/g having oxygen functional groups (e.g., COO, O, C=O) on surface. Simultaneous removal of IBP and DFS onto HTC-ZM was studied using response surface methodology with a set of 18 experiments using factors such as pH, amount of sorbent, contact time, and sorbate concentration. Maximum removal efficiency was obtained 88% and 97% for DFS and for IBP, respectively, with adsorption capacity of 2.03 mmol g-1 for DFS and 2.54 mmol g-1 for IBP. Kinetics modeling and "mean free energy" values predicted that sorption is mainly governed by physical interactions followed by "pore filling" mechanism for uptake of DFS and IBP.

The selectivity of poly(2-vinylpyridine-block-methyl methacrylate) copolymer films: an AFM study.

In this study, the surface morphologies of poly(2-vinyl pyridine-block-methyl methacrylate), P(2VP-MMA), copolymer films were analyzed by atomic force microscopy. P(2VP-MMA) samples varying in total molar mass and individual block length were evaluated for variations in the surface morphologies of films cast from toluene on Si wafers. The incorporation of AuNPs into the polymer domain significantly influenced the surface morphology of the films. Variations in the surface morphology as a function of the polarity of the casting solvent were also examined. In this context toluene (a non-polar solvent), chloroform (of intermediate polarity) and ethyl acetate (a polar solvent) were employed as casting solvents. Toluene is a good solvent for PMMA compared to P2VP, chloroform has no preferential solvation, while ethyl acetate is a good solvent for P2VP compared to PMMA. The morphology of the films cast on substrates of distinctly different polarities, such as mica, Si wafers, and HOPG, were studied to appraise their selectivity. Finally, a detailed study of the effects of thermal annealing on the surface morphologies of P(2VP-MMA) and P(2VP-MMA)-AuNPs was conducted.

Quantitative separation of hesperidin, chrysin, epicatechin, epigallocatechin gallate, and morin using ionic liquid as a buffer additive in capillary electrophoresis.

Recently, an increasing interest has been observed in ionic liquids (ILs) due to their potentialities in various chemical processes. ILs have some unique properties making them excellent additives in CE. In this work a simple, rapid, and reliable CZE method has been developed and validated using 1-butyl-3-methyl imidazolium hexafluorophosphate (BMIM-PF6 ) ionic liquid as a buffer additive for the determination/separation of five flavonoids including hesperedin, epicatechin (EC), epigallocatechin gallate (EGCG), and morin using photodiode array (PDA) detector. The effect of several parameters such as concentration and pH of the running buffer, applied voltage, and concentration of ionic liquid were optimized. CZE at 25°C with 25 mM borate buffer of pH 9.0 at an applied voltage of 17 kV by adding 17.5 mM of IL was found to be suitable for the separation/determination of all five analytes within 08 min. Validation of the method was performed in terms of linearity, accuracy, precision, and limit of detection and quantification. The calibration curves were plotted in the concentration range of 1-200 µg/mL for all five analytes. The response was linear with R2  = 0.990 for EC, chrysin, and hesperidin, 0.992 for morin, and 0.988 for EGCG. LOD and LOQ were obtained within the range of 0.4-0.5 and 1.4-1.7 µg/mL, respectively. The proposed method showed good reproducibility with RSD of less than 3% for both migration time and peak height. The method was successfully applied for the determination of flavonoids from citrus fruits and tea samples.

Ultrasonic-assisted deacetylation of cellulose acetate nanofibers: A rapid method to produce cellulose nanofibers.

Herein we report a rapid method for deacetylation of cellulose acetate (CA) nanofibers in order to produce cellulose nanofibers using ultrasonic energy. The CA nanofibers were fabricated via electrospinning thereby treated with NaOH and NaOH/EtOH solutions at various pH levels for 30, 60 and 90min assisted by ultrasonic energy. The nanofiber webs were optimized by degree of deacetylation (DD%) and wicking behavior. The resultant nanofibers were further characterized by FTIR, SEM, WAXD, DSC analysis. The DD% and FTIR results confirmed a complete conversion of CA nanofibers to cellulose nanofibers within 1h with substantial increase of wicking height. Nanofibers morphology under SEM showed slightly swelling and no damage of nanofibers observed by use of ultrasonic energy. The results of ultrasonic-assisted deacetylation are comparable with the conventional deacetylation. Our rapid method offers substantially reduced deacetylation time from 30h to just 1h, thanks to the ultrasonic energy.

2,3-Pyridine dicarboxylic acid functionalized gold nanoparticles: Insight into experimental conditions for Cr3+ sensing.

Selectivity of gold nanoparticles (AuNPs) depends upon surface functionality; small changes in structure or concentration bring significant changes in the behavior of AuNPs. In this study, citrate-capped AuNPs were functionalized with ortho-dicarboxylate substituted pyridine (2,3-PDCA) and detailed studies on experimental conditions were carried out to check the stability of AuNPs and response for Cr3+. Stability of PDCA-AuNPs was found sensitive to the pH, ionic strength of buffer and its type. Capping behavior of PDCA on C-AuNPs was examined by FTIR spectroscopy. Surface morphology and size of synthesized AuNPs were confirmed by AFM, XRD, and DLS techniques where particles were found 11nm in size, monodisperse and spherical in shape. Interaction of stabilized AuNPs was tested with various metal ions; where Cr3+ induced the changes in localized surface plasmon band (LSPR) of PDCA-AuNPs which leads to a color change from wine red to violet blue. The phenomenon is explained as cooperative effect of citrate and pyridine nitrogen on surface of AuNPs in contrary to meta-dicarboxylate substituted pyridine derivatives. Further, under optimized and controlled conditions Cr3+ shows linear response with decrease in absorbance at LSPR intensity of AuNPs (518nm). Moreover, to demonstrate the applicability of method, Cr3+ was determined in the presence of Cr (VI) which shows 96% recovery.

Gelatin-loaded p(HEMA-GMA) cryogel for high-capacity immobilization of horseradish peroxidase.

Poly(2-hydroxyethyl methacrylate-glycidyl methacrylate) [p(HEMA-GMA)] cryogel discs were prepared under sub-zero temperatures. Gelatin was attached covalently on the p(HEMA-GMA) cryogel discs and reversible immobilization of horseradish peroxidase (HRP) was performed. The p(HEMA-GMA) cryogel discs were characterized by swelling tests, scanning electron microscopy, and surface area measurements. HRP immobilization capacity of p(HEMA-GMA)/gelatin cryogel discs was 24.8 mg/g. Removal of phenol from aqueous solutions was performed using HRP immobilized p(HEMA-GMA)/gelatin cryogel. It was observed that within 2 h of contact time, the percentage of phenol removal reaches up to 91% in the presence of H2O2.

L-cysteine protected copper nanoparticles as colorimetric sensor for mercuric ions.

This report demonstrates a novel, simple and efficient protocol for the synthesis of copper nanoparticles in aqueous solution using L-cysteine as capping or protecting agent. UV-visible (UV-vis) spectroscopy was employed to monitor the LSPR band of L-cysteine functionalized copper nanoparticles (Cyst-Cu NPs) based on optimizing various reaction parameters. Fourier Transform Infrared (FTIR) spectroscopy provided information about the surface interaction between L-cysteine and Cu NPs. Transmission Electron Microscopy (TEM) confirmed the formation of fine spherical, uniformly distributed Cyst-Cu NPs with average size of 34 ± 2.1 nm. X-ray diffractometry (XRD) illustrated the formation of pure metallic phase crystalline Cyst-Cu NPs. As prepared Cyst-Cu NPs were tested as colorimetric sensor for determining mercuric (Hg(2+)) ions in an aqueous system. Cyst-Cu NPs demonstrated very sensitive and selective colorimetric detection of Hg(2+) ions in the range of 0.5 × 10(-6)-3.5 × 10(-6) mol L(-1) based on decrease in LSPR intensity as monitored by a UV-vis spectrophotometer. The developed sensor is simple, economic compared to those based on precious metal nanoparticles and sensitive to detect Hg(2+) ions with detection limit down to 4.3 × 10(-8) mol L(-1). The sensor developed in this work has a high potential for rapid and on-site detection of Hg(2+) ions. The sensor was successfully applied for assessment of Hg(2+) ions in real water samples collected from various locations of the Sindh River.

Core-shell molecularly imprinted polymer-based solid-phase microextraction fiber for ultra trace analysis of endosulfan I and II in real aqueous matrix through gas chromatography-micro electron capture detector.

In this study, core-shell molecularly imprinted polymer selective for endosulfan I and II was prepared by copolymerization of Fe3O4@SiO2-methacrylamide composites and N,N'-methylene-bis-acrylamide. The synthesized polymer was thoroughly characterized by FT-IR, TGA, and SEM. The adsorption properties of the MIP and NIP were demonstrated by equilibrium rebinding experiments, pseudo-second-order kinetic model, LF-isotherm and Scatchard analysis. The competitive recognition studies were performed with endosulfan I and II and structurally similar compounds: aldrin, dieldrin and heptachlor. The imprinting factors (IF) of endosulfan I and II were found to be 10.1 and 9.1, respectively, which were much higher than the imprinting factors (IF) of other cyclodienes. The imprinted polymer was then coated on stainless steel wire to develop an easy and simple laboratory made solid phase microextraction device for selective extraction of endosulfan I and II from water samples of environmental importance. Also the main parameters influencing coating of fiber and microextraction procedure were investigated and optimized using Plackett-Burman and Central Composite designs. The developed method was thoroughly validated for its linearity, selectivity, precision and accuracy. The developed MISPME method's linearity ranged from 7 to 5×10(3)ngl(-1) (R(2)=0.999) and from 10 to 5×10(3)ngl(-1) (R(2)=0.999) for endosulfan I and II, respectively. The limits of detection for endosulfan I and II were found to be 2ngl(-1) and 3ngl(-1), respectively. However, the limits of quantification for endosulfan I and II were 7ngl(-1) and 10ngl(-1), respectively.

LC/UV determination of cefradine, cefuroxime, and cefotaxime in dairy milk, human serum and wastewater samples.

Cephalosporins type antibiotics are widely used to treat infectious diseases. Their determination is not only important in blood/serum of patients under treatment but also in diverse matrices like wastewaters, milk etc. as contaminant. Keeping in view the need, a new high performance liquid chromatographic method for the determination of three cephalosporins (cefradine, cefuroxime and cefotaxime) has been developed. Separation was performed on an ODS column with binary solvent elution of aqueous formic acid (0.05%) and methanol in the ratio of 45: 55 (v/v) at a flow rate of 1 mL min(-1) and UV detection at 260 nm. Under optimised conditions, all three cephalosporins were baseline separated within 5 min. Linear responses for cefradine 5-20 µg mL(-1), cefuroxime 0.5-15 µg mL(-1) and cefotaxime 1.0-20 µg mL(-1) were established. LOD of 0.05-0.25 µg mL(-1) after preconcentration was achieved. The method was applied to serum samples of patients under treatment with these antibiotics and to screen the selected cephalosporins from hospital wastewater and milk samples. Moreover, method was applied to study stability of aqueous solutions and acid/base induced degradation of all three drugs.

Assay of phenolic compounds from four species of ber (Ziziphus mauritiana L.) fruits: comparison of three base hydrolysis procedure for quantification of total phenolic acids.

The present study was undertaken to investigate the flavonoid profile in four species of ber (Ziziphus mauritiana Lamk.) fruit. The 12 flavonoids identified were quercetin 3-O-robinobioside, quercetin 3-O-rutinoside, quercetin 3'-O-galactoside, quercetin 3'-O-glucoside, quercetin 3'-O-rhamnoside, quercetin 3'-O-pentosylhexoside, quercetin 3-O-6'malonylglucoside, quercetin 3'-O-malonylglucoside, luteolin 7-O-6'malonylglucoside, luteolin 7-O-malonylglucoside, myricetin 3-O-galactoside, and naringenin tri glycoside. This is the first report on extraction of nine additional flavonoids from the ber fruits. In addition, we also compared the impact of three different base hydrolysis techniques namely ultrasonic assisted base hydrolysis (UABH), microwave assisted base hydrolysis (MWABH), and pressurised liquid assisted base hydrolysis (PLABH) for the quantification of total phenolic acids. Nine phenolic acids, protocatechuic acid, p-hydroxybenzoic acid, ferulic acid, chlorogenic acid, vanillic acid, caffeic acid, vanillin, ortho- and para-coumaric acids, were identified and quantified. The three major phenolic acids identified in all four ber species were p-coumaric acid, vanillin and ferulic acids. Higher amounts (p<0.05) of total phenolic acids in all cultivars were obtained with the PLABH technique as compared to other two procedures (UABH and MWABH).

Single-channel flow injection spectrophotometric determination of nickel using furildioxime in micellar solution.

A very simple, selective, and fast flow injection spectrophotometeric method is developed for determination of nickel using furildioxime as complexing agent. Micellar solution of brij-35 is employed to solubilize the sparingly soluble complex of Ni-furildioxime in buffered aqueous system (pH-9.00). Under optimized conditions, absorbance is linear from 0.02 to 10 µg mL(-1) using 500 µL sample volume and from 10 to 30 µg mL(-1) using 50 µL sample volume of nickel at 480 nm, with R(2) = 0.9971 and 0.9916, respectively. The molar absorption coefficient and Sandell's sensitivity were 6.0 × 10(3) L mol(-1) cm(-1) and 0.01 ng cm(-2), respectively. The sample throughput of the method is 120 samples per hour with RSD of 0.01-0.2% for 0.02 to 10 µg mL(-1) nickel (n = 5), indicating that the method is highly precise and reproducible. Interference from cobalt is removed by Nitroso R-salt-modified XAD-16. The developed method is validated by analysing certified reference materials and is applied to assess nickel content of commercially available cigarettes.

Preparation and characterization of molecularly imprinted polymer for di(2-ethylhexyl) phthalate: application to sample clean-up prior to gas chromatographic determination.

The molecularly imprinted polymer (MIP) selective for di(2-ethylhexyl) phthalate (DEHP) an environmental endocrine disruptor was prepared by suspension polymerization using methacrylamide as functional monomer and N,N'-methylene-bis-acrylamide as cross-linker. The imprinted polymer was employed for solid-phase extraction of DEHP from water samples of environmental importance and characterized by FT-IR and SEM. The adsorption properties of the imprinted polymer were demonstrated by equilibrium rebinding experiments, Pseudo-second-order kinetic model, Sips isotherm and Scatchard analysis. The reusability of MIP was checked for at least six repeated batch adsorption cycles and the results showed almost no deterioration in the adsorption capacity. The competitive recognition studies were performed with DEHP and structurally similar compounds; dimethyl phthalate (DMP), diethyl phthalate (DEP), and dibutyl phthalate (DBP). The imprinting factor (IF) of DEHP was found to be 12.86 which was much higher than the imprinting factors (IF) of other phthalates. A method constituted by molecularly imprinted solid-phase extraction (MISPE) with GC-FID was developed for DEHP analysis in water samples under very simple conditions. Sample loading and desorption conditions were also optimized. The MISPE method's linearity ranged from 0.035 to 3.0 µg ml⁻¹ with r² = 0.9998. Intra-assay, interassay precision and accuracy ranged from 0.0168% to 1.017%, 1.130% to 4.799% and 94.98% to 99.35%, respectively. The LOD and LOQ were found to be 0.011 and 0.035 µg ml⁻¹, respectively. Synthesized MIP was employed in MISPE for cleaning up the spiked river water samples prior to gas chromatographic analysis. The river samples were found to contain DEHP in the range of 1.4 × 10⁻³ to 0.349 µg ml⁻¹.