Determination of Carbamate Pesticide Residues in Vegetables and Fruits by Liquid Chromatography-Atmospheric Pressure Photoionization-Mass Spectrometry and Atmospheric Pressure Chemical Ionization-Mass Spectrometry

Yokogawa Analytical Systems Inc, 3-3-11 Niitaka, Yodogawa-ku, Osaka 532-0033, Japan.
Journal of Agricultural and Food Chemistry (Impact Factor: 2.91). 03/2004; 52(4):727-35. DOI: 10.1021/jf0343377
Source: PubMed


A liquid chromatography-atmospheric pressure photoionization (APPI)-mass spectrometry method was developed for the determination of 22 carbamates including their metabolites in vegetables and fruits. For the optimization of APPI, several APPI ion source parameters were examined. As a result, many carbamates with APPI using the optimized parameter gave simple mass spectra, and a strong signal corresponding to [M + H](+) was observed except for aldicarb. However, some carbamate metabolites gave ammonium adduct ions [M + NH(4)](+) as base peak ions. The mean recovery of each carbamate from grape and onion samples spiked at 5 ng/g was 81.7-105.7%, with relative standard deviations of 3.3-5.9%. Furthermore, matrix constituents did not significantly influence the ionization efficiency. The limit of detection (S/N = 3) in grape and onion was in the range of 0.33-3.33 ng/g. For the robustness of this method, this system has been used to analyze 50 samples, and the intensities for all carbamates were found to be unaffected by the contamination of the APPI source by sample matrix constituents. This result indicates that the method is reliable.

63 Reads
  • Source
    • "The APPI mass spectra of organochlorine pesticide p,p 0 dichlorodiphenyltrichloroethane (DDT) (Moriwaki & Miyakoda, 2007), hexachlorobenzene (Osaka et al., 2009) and the effect of dopant on their ionization was described. The determination of carbamate pesticides using LC–APPI–MS were effectively carried out with sensitivities comparable to that of APCI method (Takino et al., 2004). Apart from these methods , the APPI technique is not explored to its potential for the analysis of pesticide residues when compared to the other methods. "
    [Show abstract] [Hide abstract]
    ABSTRACT: A novel analytical method was developed for determination of organochlorine, synthetic pyrethroid, organophosphate and carbamate pesticide residues in fruit juices using ultra performance liquid chromatography–atmospheric pressure photoionization–high resolution mass spectrometry (UPLC– APPI–HRMS). The analytes were extracted from fruit juices by dispersive solid-phase extraction using multi-walled carbon nanotubes (MWCNTs). The analysis was carried out in full scan mode using dual ionization mode of APPI in the mass range of 100–650 units. The limit of detection and limit of quantification values for the pesticides were in the range of 0.025–0.15 ng/mL and 0.1–0.5 ng/mL respectively. The matrix effect of the method was found to be low and extraction recoveries were in the range of 60–110%. Some of the real fruits juice samples showed the presence of some pesticides in the range of 6.5–24.8 ng /L.
    Full-text · Article · Nov 2014 · Food Chemistry
  • Source
    • "In the laboratory, the analytical procedure used involved solvent extraction of homogenized samples, clean-up on a solid phase extraction column and analysis using reversephase high performance liquid chromatography (HPLC) with an ultra violet (UV) detector. This procedure was chosen after a review of previous methods available in literature (Argauer et al. 1995; Lalah and Wandiga 1996; Yang et al. 1996; Pogacnik and Franko 1999; Kawamoto and Makthata 2003; Takino et al. 2004; Vyas et al. 2005). Accurately weighed 25 g, separately, of weathered feet and beaks of the dead birds were cut into small pieces using a pair of scissors. "
    [Show abstract] [Hide abstract]
    ABSTRACT: Forensic analysis of carbofuran residues in weathered tissue samples for evidence of Furadan exposure in vultures (Gps africanus) by HPLC gave concentration (mg/Kg dry tissue weight) ranges of bdl - 0.07 (carbofuran), bdl - 0.499 (3-ketocarbofuran) and 0.013-0.147 (3-hydroxycarbofuran) in beaks, bdl-0.65 (carbofuran), 0.024-0.190 (3-ketocarbofuran) and 0.017-0.098 (3-hydroxycarbofuran) in feet, 0.179-0.219 (3-ketocarbofuran) and 0.081-0.093 (3-hydroxycarbofuran) in crop content, 0.078-0.082 (3-ketocarbofuran) and 0.091-0.101 (3-hydroxycarbofuran) in muscle of a laced carcass and 0.006-0.014 (carbofuran), 0.590-1.010 (3-ketocarbofuran) and 0.095-0.135 (3-hydroxycarbofuran) in soil sampled from a poisoning site. These compounds were confirmed by GC-MS. The results showed that HPLC combined with GC-MS is suitable for forensic analysis of carbofuran residues in bird tissue samples and that forensic investigation should include its two toxic metabolites, 3-hydroxycarbofuran and 3-ketocarbofuran.
    Full-text · Article · Apr 2010 · Bulletin of Environmental Contamination and Toxicology
  • Source
    • "This procedure was chosen after review of previous methods available in literature. [18] [21] [27] [28] The soil samples were air-dried overnight in the laboratory at room temperature in darkness then 25 grams weighed. To achieve satisfactory recovery, samples were further dried by mixing, separately, with 20 g of anhydrous sodium sulphate before homogenization in a mortar with pestle followed by sieving through a 2-mm mesh. "
    [Show abstract] [Hide abstract]
    ABSTRACT: This study was undertaken to determine the concentrations of carbofuran residues in water, soil and plant samples from selected sites in the farmlands in Kenya and to demonstrate the impact of Furadan use on the local environment. Soil, water and plant samples obtained from agricultural farmlands where the technical formulation Furadan has been used extensively showed high environmental contamination with concentrations of carbofuran and its two toxic metabolites 3-hydroxycarbofuran and 3-ketocarbofuran, separately, ranging from 0.010-1.009 mg/kg of dry surface soil, 0.005-0.495 mg/L in water samples from two rivers flowing through the farms and bdl-2.301 mg/L in water samples from ponds and dams located close to the farms. Maize plant samples contained these residues in concentrations ranging from 0.04-1.328 mg/kg of dry plant tissue. The significantly high concentration levels of carbofuran and its metabolites, 3-ketocarbofuran and 3-hydroxycarbofuran, found in various matrices demonstrate that Furadan was used extensively in the two areas and that there was environmental distribution and exposure of residues in water which posed risks when used for domestic purposes or as drinking water for animals in two wildlife conservancies where the dams and ponds are located. Surface soil contamination was also high and posed risks through run-off into the dams and rivers as well as through secondary exposure to small birds and mammals.
    Full-text · Article · Feb 2010 · Journal of Environmental Science and Health Part B Pesticides Food Contaminants and Agricultural Wastes
Show more