Aree Choodum

Rapid and semi-quantitative presumptive tests for opiate drugs

Digital image analysis was applied to the products of simple colour presumptive tests for opiates. Adobe Photoshop software was used for colour analysis to obtain analytical data in the form of a Red Green Blue (RGB) value. Calibration curves were developed for morphine, codeine, and diamorphine hydrochloride and the developed tests successfully applied to seized heroin samples to demonstrate the application of the technique in a forensic case context. Good agreement with gas chromatographic quantification results was obtained for the illicit samples analysed and a wide linear range and low detection limit for all drugs under test facilitated the application to illicit samples. The results show great potential for use as a semi-quantitative field test for illicit drug compounds.

Rapid quantitative colourimetric tests for trinitrotoluene (TNT) in soil

A rapid quantitative colourimetric test was developed for the determination of 2,4,6-Trinitrotoluene (TNT) in soil. Quantification was achieved using an innovative application of photography where the relationship between the Red Green Blue (RGB) value and concentration of colorimetric product was exploited. The wide linear range (1-50 mg/L) and low detection limit (0.73±0.01 mg/L to 3.5±0.4 mg/L) achieved was comparable with spectrophotometric quantification methods. Quantification was validated both with known concentration standards and spiked soil extracts confirming the accuracy of the technique. The results demonstrate a powerful technique with the capacity for development as a rapid on site field test for the analysis of explosives.

Real time quantitative colourimetric test for methamphetamine detection using digital and mobile phone technology

The Simon presumptive color test was used in combination with the built-in digital camera on a mobile phone to detect methamphetamine. The real-time Red-Green-Blue (RGB) basic color data was obtained using an application installed on the mobile phone and the relationship profile between RGB intensity, including other calculated values, and the colourimetric product was investigated. A wide linear range (0.1-2.5mg mL(-1)) and a low detection limit (0.0110±0.0001-0.044±0.002mg mL(-1)) were achieved. The method also required a small sample size (20μL). The results obtained from the analysis of illicit methamphetamine tablets were comparable to values obtained from gas chromatograph-flame ionization detector (GC-FID) analysis. Method validation indicated good intra- and inter-day precision (2.27-4.49%RSD and 2.65-5.62%RSD, respectively). The results suggest that this is a powerful real-time mobile method with the potential to be applied in field tests.

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.

Smart phone: A popular device supports amylase activity assay in fisheries research

Colourimetric determinations of amylase activity were developed based on a standard dinitrosalicylic acid (DNS) staining method, using maltose as the analyte. Intensities and absorbances of red, green and blue (RGB) were obtained with iPhone imaging and Adobe Photoshop image analysis. Correlation of green and analyte concentrations was highly significant, and the accuracy of the developed method was excellent in analytical performance. The common iPhone has sufficient imaging ability for accurate quantification of maltose concentrations. Detection limits, sensitivity and linearity were comparable to a spectrophotometric method, but provided better inter-day precision. In quantifying amylase specific activity from a commercial source (P>0.02) and fish samples (P>0.05), differences compared with spectrophotometric measurements were not significant. We have demonstrated that iPhone imaging with image analysis in Adobe Photoshop has potential for field and laboratory studies of amylase.

On-site semi-quantitative analysis for ammonium nitrate detection using digital image colourimetry

Digital image colourimetry was successfully applied in the semi-quantitative analysis of ammonium nitrate using Griesss test with zinc reduction. A custom-built detection box was developed to enable reproducible lighting of samples, and was used with the built-in webcams of a netbook and an ultrabook for on-site detection. The webcams were used for colour imaging of chemical reaction products in the samples, while the netbook was used for on-site colour analysis. The analytical performance was compared to a commercial external webcam and a digital single-lens reflex (DSLR) camera. The relationship between Red-Green-Blue intensities and ammonium nitrate concentration was investigated. The green channel intensity (IG) was the most sensitive for the pink-violet products from ammonium nitrate that revealed a spectrometric absorption peak at 546 nm. A wide linear range (5 to 250 mgL⁻¹) with a high sensitivity was obtained with the built-in webcam of the ultrabook. A considerably lower detection limit (1.34 ± 0.05mgL⁻¹) was also obtained using the ultrabook, in comparison with the netbook (2.6 ± 0.2 mgL⁻¹), the external web cam (3.4 ± 0.1 mgL⁻¹) and the DSLR (8.0 ± 0.5 mgL⁻¹). The best inter-day precision (over 3 days) was obtained with the external webcam (0.40 to 1.34%RSD), while the netbook and the ultrabook had 0.52 to 3.62% and 1.25 to 4.99% RSDs, respectively. The relative errors were +3.6, +5.6 and -7.1%, on analysing standard ammonium nitrate solutions of known concentration using IG, for the ultrabook, the external webcam, and the netbook, respectively, while the DSLR gave -4.4% relative error. However, the IG of the pink-violet reaction product suffers from interference by soil, so that blank subtraction (|IG-IGblank| or |AG-AGblank|) is recommended for soil sample analysis. This method also gave very good accuracies of -0.11 to -5.61% for spiked soil samples and the results presented for five seized samples showed good correlations between the various imaging devices and spectrophotometer used to determine ammonium nitrate concentrations. Five post-blast soil samples were also analysed and pink-violet product were observed using Griesss test without zinc reduction indicating the absence of ammonium nitrate. This demonstrates significant potential for practical and accurate on-site semi-quantitative determinations of ammonium nitrate concentration.

A comprehensive chromatographic comparison of amphetamine and methylamphetamine extracted from river water using molecular imprinted polymers and without the need for sample derivatization

This work explores the differences between two GCMS instruments for the determination of amphetamine and methylamphetamine extracted from water samples (ultra pure water and river water) without the necessity for derivatization. The instruments contained different generations of gas chromatograph and mass selective detector components and revealed significantly different results when presented with the same samples. The extraction methodology also compared two SPE systems. The extraction efficiency of commercially available molecular imprinted polymers as a sorbent in SPE was compared with commonly used hydrophilic balance sorbent. Molecular imprinted polymers provided excellent recoveries (81 ± 2% and 108 ± 3% at 30 μg L(-1), and 94 ± 2% and 94 ± 2% at 200 μg L(-1) for amphetamine and methylamphetamine, respectively). The best LOD obtained was sufficient for the determination of both drugs extracted from river water (0.029 ± 0.003 and 0.015 ± 0.004 μg L(-1) for amphetamine and methylamphetamine, respectively). These were comparable to literature values obtained through conventional extraction and analysis using LC-MS/MS but had the advantage of being achieved using an underivatized GCMS method.

Fluorinated monolithic column for CEC.

In order to overcome the drawbacks associated with particle-based fluorinated stationary phases, a fluorinated cationic monolith was successfully synthesized by the in situ copolymerization of a 45% monomer mixture and 55% porogens with thermal initiation using 0.1% initiator with respect to the monomer mixture. The monomer mixture was composed of perfluorododecyl acrylate (49.75%), ethylene dimethacrylate (49.75%), and 0.5% of the quaternary amine acrylic monomer supporting an anodal electroosmotic flow. A tertiary porogenic solvent system consisting of 40% 1-propanol, 40% 1-octanol, and 20% 1-dodecanol was used. The resulting monolith column showed good characteristics in terms of morphology, permeability (pressure drop was 4.8-25.7 MPa between 5 and 25 μL/min), and the electroosmotic mobility (3.68 (±0.05)×10(-4) cm(2) v(-1) s(-1)). The monolith was tested for the separation of four phenolic compounds, three aromatic hydrocarbons, and one fluorine-containing compound. Good efficiencies (up to 135,000 (±4000) plate/m and resolution up to 2.6 (±0.1)) with short analysis time (< 9 min for tau-fluvalinate, <7 min for four phenolic compounds, and <12 min for three aromatic hydrocarbons) and good stability (1.0-1.5% RSD for intraday, 1.2-1.6% RSD for interday, and 3.9-5.0% RSD for column-to-column) were obtained.

A cost effective hydrogel test kit for pre and post blast trinitrotoluene

A cost effective hydrogel test kit was successfully developed for the detection of pre- and post-blast trinitrotoluene (TNT). A polyvinyl alcohol (PVA) hydrogel matrix was used to entrap the potassium hydroxide (KOH) colourimetric reagent. The easily portable test kit was fabricated in situ in a small tube to which the sample could be added directly. The test kit was used in conjunction with digital image colourimetry (DIC) to demonstrate the rapid quantitative analysis of TNT in a test soil sample. The built-in digital camera of an iPhone was used to capture digital images of the colourimetric products from the test kit. Red-Green-Blue (RGB) colour data from the digital images of TNT standard solutions were used to establish a calibration graph. The validation of the DIC method indicated excellent inter day precision (0.12-3.60%RSD) and accuracy (93-108% relative accuracy). Post-blast soil samples containing TNT were analysed using the test kit and were in good agreement with spectrophotometric analysis. The intensity of the RGB data from the TNT complex deviated by +6.3%, +5.1%, and -4.9% after storage of the test kits in a freezer for 3 months. The test kit was also reusable for up to 12 times with only -5.4%, +0.3%, and +4.0% deviations. The hydrogel test kit was applied in the detection of trace explosive residues at the scene of the recent Bangkok bombing at the Ratchaprasong intersection and produced positive results for TNT demonstrating its operational field application as a rapid and cost effective quantitative tool for explosive residue analysis.

Portable and selective colorimetric film and digital image colorimetry for detection of iron

Iron is an important trace element in environmental and biological systems, the development of simple and selective methods for the determination of iron is important. In this work, completely biodegradable tapioca starch was introduced as the substrate to entrap standard chromogenic probes (1,10-phenanthroline) for fabrication of a novel colorimetric sensor for ferrous. A clear plasticized thin film from tapioca starch was fabricated inside a small plastic tube as a portable test kit. A red complex was obtained by exposing the film to a ferrous solution, while no color changes were obtained with various other ions, indicating excellent selectivity. The developed films were applied in conjunction with a digital image colorimetry for quantification of ferrous. Calculated molecular absorption of the red complex showed the widest linear range (0 to 10 mg L-1) with good linearity (R2 < 0.9934) with ferrous concentrations. The developed method provided good inter-day precision (1.75 to 3.97%RSD, 5 days 15 sensors), good accuracy (+2.35% to +4.57% relative error), and low detection limit (0.09 ± 0.01 mg L-1). The concentrations of ferrous ion in soil and water samples quantified by the developed method were not significantly different from atomic absorption spectrophotometry at 95% confidence level. The films were stable for at least three months.