Molecularly imprinted polymer for analysis of trace atrazine herbicide in water

A molecularly imprinted polymer (MIP) for atrazine was synthesized by non-covalent method. The binding capacity of MIP was 1.00 mg g^{? 1} polymer. The selectivity and recovery were investigated with various pesticides which are mostly, found in the environment, for both similar and different chemical structure of atrazine. The competitive recognition between atrazine and structurally similar compounds was evaluated and it was found that the system provided highest recovery and selectivity for atrazine while low recovery and selectivity were obtained for the other compounds. The highest recovery was obtained from MIP compared with non-imprinted polymer (NIP), a commercial C₁₈ and a granular activated carbon (GAC) sorbent. The method provided high recoveries ranged from 94 to 99% at two spiked levels with relative standard deviations less than 2%. The lower detection limit of the method was 80 ng L^{? 1}. This method was successfully applied for analysis of environmental water samples.     

Acetaldehyde residue in polyethylene terephthalate (PET) bottles

A simple sample preparation technique was developed for rapid analysis of acetaldehyde residue in Polyethylene Terephthalate (PET) bottles. A laboratory-built heating system was used and coupled with gas chromatography-flame ionization detector (GC-FID) at optimized conditions. The results were a tremendous reduction of the sample preparation time from 24 hours, for the conventional method, to only one hour. The analysis took only 1.5 min with other good analytical performances i.e. a low detection limit, 0.3 ng mL^{? 1} and a wide linear dynamic range, 0.3 ng mL^{? 1} to 6.6 μ g mL^{? 1} with R² > 0.99.Acetaldehyde residue in freshly blown bottles were analyzed and found in the range of 0.4 to 1.1 ng mL^{? 1}. The results were good agreement with the conventional 24-hour airspace method (P < 0.01). The PET-bottle sampling technique was also developed to minimize the complication of sample transportation and pre-concentration. A purge and trap technique was found to be the most suitable. Then, it was implemented and compared, the results showed no significant difference (P < 0.01) with and without purge and trap.     

Development of an in-line system for the analysis of 4,4'-DDT in water

An in-line system for trace persistent organic pollutants (POPs) in water was developed by using a laboratory-made hollow fiber membrane (HFM) unit connected with a high-resolution gas chromatograph-mass spectrometer (HRGC-MS). The semivolatile organic compound, 4,4'-Dichlorodiphenyl trichloroethane (4,4'-DDT), was chosen as a representative of a persistent organic compound. The synthetic water contaminated with 4,4'-DDT was passed through the HFM unit, the extraction occurred by the analyte pervaporated and permeated, then stripped into HRGC-MS. Several factors were investigated for the high extraction efficiency. The best performance was obtained at sample and stripping gas flow rates of 6 and 9 mLmin-1, respectively, and desorption temperature of 60 degrees C. At this temperature, the diffusion rate was enhanced by 15 times over 25 degrees C. A wide linear dynamic range was obtained, i.e., 0.10-1.0 mgL-1, with a limit of detection (LOD) of 90 microgL-1. The extraction efficiency of 4,4'-DDT in real water samples was in the range of 83-94%. Real water samples were analyzed and 0.6 microgL-1 of 4,4'-DDT was found in unregistered bottled water and 7.0 microgL-1 in tap water.     

Organochlorine pesticide residues in Songkla Lake

The water quality of Songkla Lake for organochlorine (OC) pesticide contamination was studied from chosen sampling sites (stations) using the lakes geographic data and pollution sources. The water samples were collected monthly from 13 stations in Songkla Lake during September 1991–November 1992. The OC pesticide residues found were Heptachlor, Heptachlor Epoxide, DDD, DDE, DDT and Aldrin in the range 0–0.5690 ppm. This study showed that DDT and its metabolite products (DDD and DDE) dominated OC pesticide residues in the lake. The concentration of OC residues also depended on the season, i.e. at some sampling stations the concentration of OC residues in the dry season (July–September) were higher than in the wet season (October–January).     

A miniature stainless steel net dumbbell-shaped stir-bar for the extraction of phthalate esters in instant noodle and rice soup samples

Abstract

This work reports the development of a very-simple-to-construct stir-bar extraction device so called “a dumbbell-shaped stainless steel stir-bar.” The extraction device was assembled from a rolled up stainless steel net filled with an XAD-2 sorbent and a metal rod to allow the use of a magnetic stirrer during extraction. The dumbbell-shaped stainless steel stir-bar was used to extract diethyl phthalate (DEP), dibutyl phthalate (DBP), and di(2-ethylhexyl) phthalate (DEHP) before analysis by a gas chromatograph equipped with an electron capture detector (GD-ECD). Under the optimal conditions, the developed method provided a good linearity from 10.0 to 1,000.0?ng mL^?1 for all three compounds. Limits of detection and limits of quantification were 9.37?±?0.29?ng mL^?1 and 31.22?±?0.95?ng mL^?1 for DEP, 5.73?±?0.31?ng mL^?1 and 19.1?±?1.0?ng mL^?1 for DBP and 3.30?±?0.06?ng mL^?1 and 11.0?±?0.19?ng mL^?1 for DEHP, respectively. Good recoveries in the range of 81.89?±?0.17 to 109.5?±?2.0% were achieved when the method was used to extract phthalate esters in five instant noodle and two rice soup samples.     

Trace phthalate and adipate esters contaminated in packaged food

A method for trace analysis of two plasticizers, di-2-ethylhexyl phthalate (DEHP) and di-2-ethylhexyl adipate (DEHA), contaminated in packaged curry paste were investigated by gas chromatography with flame ionization detector (GC-FID). Curry paste samples were extracted by ultrasonic and solid phase extraction using Florisil® cartridge. Analysis by the GC-FID system provided limits of detection for DEHA and DEHP at 12 and 25 μ g L^{? 1} and a linear dynamic range between 25 μ g L^{? 1} to 60 mg L^{? 1} with a coefficient of determination (R²) greater than 0.99. High recoveries were obtained, ranged from 91 to 99% and 88 to 98% for DEHP and DEHA with RSD lower than 7 and 10% respectively. The method detection limit and limits of quantitation were ranged from 27 to 30 and 90 to 100 μ g L^{? 1}. The analysis of curry paste samples showed concentrations of DEHP and DEHA in the range of 4.0 ng g^{? 1} to 0.61 μg g^{? 1}.     

Some gaseous pollutants in Nakorn Sri Thammarat

Three gaseous pollutants, carbon monoxide, nitrogen dioxide, and sulfur dioxide were studied in the Nakorn Sri Thammarat Province area (Thailand) during March-August 1987. Air samples were taken from 12 stations covering four districts, i.e., Tungsong, Pakpanang, Muang, and Kanoum. Five stations are located in areas of light traffic conditions and low human population and seven are in densely populated areas with heavy traffic conditions.In this study the concentrations of pollutants found were in the range of non-detectable-0.7 ppm for carbon monoxide, 0.6–7.4 pphm for nitrogen dioxide, and non-detectable-7.4 pphm for sulfur dioxide.     

Online microchannel preconcentrator for carbofuran detection

A simple and rapid online microchannel preconcentrator coupled with an amperometric detection for the analysis of carbofuran using polyethylene glycol coated onto magnetic particle (PEG-magnetic particles) sorbents was developed. This simple-to-prepare microchannel preconcentrator used an external magnet to retain the PEG-magnetic particle sorbents inside the microchannel. Under optimum conditions, the system provided two linear ranges, from 0.01 to 10.0 mg L^?1 and from 10.0 to 130.0 mg L^?1 with a limit of detection of 8.7 ± 0.1 μg L^?1. The microchannel preconcentrator provided very good stability; it can be used for up to 326 consecutive injections of 5.0 mg L^?1 carbofuran with a relative standard deviation of less than 3%. The developed system provided a good microchannel-to-microchannel and a good electrode-to-electrode reproducibility (n = 6, %RSD < 1). It also provided an excellent selectivity when it was tested with two other carbamate pesticides, carbaryl and methomyl, with a 43 and 256 times higher detection sensitivity for carbofuran, respectively. The developed system was successfully applied to detect carbofuran in surface water samples obtained near vegetable plantation areas. The concentrations of carbofuran in these samples were found to be in the range of non-detectable to 0.047 ± 0.001 mg L^?1. The developed system is easy to operate and easy to couple with other analytical instruments and it could be easily adapted for the analysis of other polar organic contaminants.     

Capillary microextraction for simultaneous analysis of multi-residual semivolatile organic compounds in water

Capillary microextractor (CME) in combination with a gas chromatograph-mass spectrometer (GC-MS) was employed for the determination of trace priority hazardous substances in water. Three groups of semivolatile organic compounds (SVOCs), i.e., chlorinated hydrocarbons, pesticides and polycyclic aromatic hydrocarbons (PAHs), were simultaneously determined. SVOCs were extracted from 7 mL of water samples on a 100 cm commercial gas chromatographic column (0.32 mm id x film thickness 0.25 microm, HP-5 capillary column) and eluted with only 3 microL of acetonitrile. The extractant was analyzed by GC-MS in the selected ion monitoring mode. The method showed good linearity over the concentration range 10 ng L(-1) to 3.0 mg L(-1) with correlation coefficients (r) greater than 0.99 and low limits of detection ranged from 10 ng L(-1) to 1.0 mg L(-1). High recovery (more than 80%) was obtained with relative standard deviation less than 10%. The method was successfully applied for trace level analyses of SVOCs in water samples.     

Trace phthalate and adipate esters contaminated in packaged food

A method for trace analysis of two plasticizers, di-2-ethylhexyl phthalate (DEHP) and di-2-ethylhexyl adipate (DEHA), contaminated in packaged curry paste were investigated by gas chromatography with flame ionization detector (GC-FID). Curry paste samples were extracted by ultrasonic and solid phase extraction using Florisil(R) cartridge. Analysis by the GC-FID system provided limits of detection for DEHA and DEHP at 12 and 25 microg L(- 1) and a linear dynamic range between 25 microg L(- 1) to 60 mg L(- 1) with a coefficient of determination (R(2)) greater than 0.99. High recoveries were obtained, ranged from 91 to 99% and 88 to 98% for DEHP and DEHA with RSD lower than 7 and 10% respectively. The method detection limit and limits of quantitation were ranged from 27 to 30 and 90 to 100 microg L(- 1). The analysis of curry paste samples showed concentrations of DEHP and DEHA in the range of 4.0 ng g(- 1) to 0.61 microg g(- 1).