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1.
Anal Chem ; 78(11): 3752-7, 2006 Jun 01.
Article in English | MEDLINE | ID: mdl-16737233

ABSTRACT

Environmental and security applications have generated major demands for effective field-deployable tools for detecting nitroaromatic compounds, such as chloramphenicol (an antibiotic), parathion (an organophosphate nerve agent), and TNT (2,4,6-trinitrotoluene, an explosive) in a fast, simple, sensitive, reliable, and cost-effective manner. We report here a single-run approach for such a purpose. The reduction potential of different nitroaromatic compounds was found to systematically shift with the substituent group at an electrochemically preanodized screen-printed carbon electrode. The preanodization treatment makes the peak sharp and hence provides a precise way to identify the substituent effect on nitroaromatic compounds. By using potential shifts as analytical characteristics of nitroaromatic compounds, a suitable internal standard can be chosen based on the criteria of well-separated peak potential and rarely found in the real sample of interest. Simply by measuring the ratio of peak currents between analytes of interest and internal standard, the analysis can be done in a single-run measurement. Both the matrix effect and the variation of electrode during the preparation process can be canceled out in this approach and thus allows for a high-precision analysis. Just by placing a 20-microL drop on a single-use amperometric sensor strip incorporating a three-electrode configuration is enough for rapid and sensitive detection of nitroaromatic compounds by square-wave voltammetry. For example, the linear detection range can be up to 100 microM with a detection limit of 0.42 microM (S/N = 3) in the detection of chloramphenicol. This approach was successfully demonstrated in real sample analysis to verify the applicability of the method. The promising performances open new possibilities for rapid determination of nitroaromatic compounds in environmental and biological samples.


Subject(s)
Nitrogen Compounds/analysis , Nitrogen Compounds/chemistry , Calibration , Electrochemistry , Electrodes , Molecular Structure , Water
2.
J Pharm Biomed Anal ; 41(4): 1332-41, 2006 Jun 16.
Article in English | MEDLINE | ID: mdl-16621415

ABSTRACT

A sensitive enzyme-linked immunosorbent assay (ELISA) was developed for the detection of fentanyl in serum and urine. The ELISA used an indirect competitive method produced by coating the plate with thyroglobulin conjugated with fentanyl hapten. Antibodies against fentanyl-hemocyanin were detected by a goat-anti-rabbit antibody conjugated with alkaline phosphatase. Calibration standard curves ranged from 0.5ng/ml to 50mug/ml (IC(50)=10ng/ml), and the limits of detection were 0.5 and 1.0ng/ml for serum and urine, respectively. The intra- and inter-assay variations were less than 8% and 10%, respectively. The antibody produced against fentanyl completely cross-reacted with p-fluorofentanyl, thienylfentanyl and 3-methylthienylfentanyl, cross-reacted highly with carfentanil (85%), but was considered non-cross-reactive with alpha-methylfentanyl (5%), sufentanil (<1%), alfentanil (<1%) and lofentanil (<1%). Nano-sized iron oxide magnetic particles coated with the developed fentanyl antibody were capable of specific binding and releasing of fentanyl from urine samples. This enabled the drug to be effectively pre-concentrated and decreased the limit of detection by approximately one order of magnitude. The analytical background noise was significantly reduced to enable fentanyl detection at concentrations originally below chromatographic limit of detection. The change of platform for antibody binding with nanoparticles demonstrated a novel use of antibodies for sample preparation and should facilitate drug screening by traditional ELISA.


Subject(s)
Adjuvants, Anesthesia/urine , Antibodies/metabolism , Fentanyl/urine , Adjuvants, Anesthesia/blood , Adjuvants, Anesthesia/metabolism , Animals , Anti-Bacterial Agents/urine , Cross Reactions , Electrophoresis, Capillary/methods , Enzyme-Linked Immunosorbent Assay/methods , Fentanyl/analogs & derivatives , Fentanyl/metabolism , Horses , Nanostructures , Rabbits
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