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A simple method for the simultaneous determination of dihydrostreptomycin, spectinomycin, spiramycin, streptomycin, tilmicosin, and tylosin in meat has been developed using pressurized liquid extraction and LC-triple quadrupole MS (LC-ESI-MS/MS). The pressurized liquid extraction operational parameters were optimized and no protein precipitating and fat removing steps were required. A gradient HPLC separation was developed with ion-pair mobile phases consisting of aqueous 1 mM heptafluorobutyric acid water and methanol. Protonated molecules were used as precursor ions for CID. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring of three fragment ion transitions to provide a high degree of sensitivity and specificity. Dirithromycin and sisomycin were selected as internal standards. A validation study was conducted for these antibiotics in poultry meat samples. All selected compounds could be detected (monitoring ions by multiple reaction monitoring) in meat samples at amounts below the regulatory level of concern. Using the internal standards, pressurized liquid extraction recovery rates were from 70 to 96% (RSD 12-25%). LC-ESI-MS/MS method detection limits of the selected antibiotics were 1-6 microg/kg. Good method reproducibility was found by intra- and inter-day precisions at maximum residue level, yielding the RSDs less than 15 and 16%, respectively.

The occurrence of aflatoxins (AFs) in dried fruits and nuts available in Rabat-Sale area (Morocco) was surveyed in this study. One hundred samples of dried fruits and nuts, purchased from retail shops and local markets from January to October 2006, were analyzed for AFs content by immunoaffinity (IAC) clean-up with liquid chromatography and fluorescence detection. Results showed that the incidences of total aflatoxins (AFT) and aflatoxin B1 (AFB1) in peanut, dried raisins, dried figs, walnut, and pistachio were 5%, 20%, 30%, 30% and 45% and 5%, 20%, 5%, 30% and 45%, respectively. The highest contamination levels of AFB1 were found in one walnut sample (2500 μg/kg) and one pistachio sample (1430 μg/kg). 5%, 20% and 20% of samples of pistachio, walnut and dried raisins exceeded the maximum tolerable limit (2 μg/kg) set for AFB1 by EU regulations. While 15% of dried figs samples were above the maximum limit (4 μg/kg) set by EU regulations for AFT. The present paper is the first report on the natural occurrence of AFs in dried fruits and nuts available in Rabat-Sale area in Morocco.

Graphitized Carbon Black (GCB) extractive cartridges are evaluated for on-line coupling with a C8 analytical column to determine eleven carbamates and one carboximide pesticide from spiked deionized water at the 1.2 μg/L level. Several experiments were carried out to ascertain whether GCB saturation, pesticide degradation on the surface, existence of by-pass channels, mobility among the bulk cartridge, or strong retention on the surface interfere with the determination of pesticides. Problems in on-line CGB elution are partially solved by modifying the acetonitrile/water gradient to contain a front of 100% acetonitrile for a few seconds. Eluting the same GCB cartridges off-line with dichloromethane/methanol gives recoveries higher than 77% for the selected pesticides.

The application of SPE technology to the isolation of pesticides and related compounds from food and soils has grown enormously in the last decade. Much of this growth has been due to the relative ease of sample handling and the wide range of solid supports currently available for a variety of applications. The aim of this review is to present the methods for solid phase extraction (SPE) of pesticide residues from soils and foods. There are three main areas according to the type of approach used to handle the sample: solid phase extraction, solid phase clean-up (SPC), and matrix solid phase dispersion (MSPD). This review covers milk products, fatty foods, fruits, vegetables, and soils. Solid phase materials are discussed in each case in terms of reversed bonded-phase silica sorbents (C18, C8, C2, etc.) and polar sorbents (alumina, Florisil, and silica).

A method for polychlorinated biphenyl (PCB) trace extraction from contaminated water at the part-pertrillion levels is described. This procedure involves quantitative adsorption of PCBs on Cis glass microcolumns. PCBs are retained on the surface and subsequently eluted with n-hexane (5 mL) before gas chromatography. Recovery of water fortified with PCBs was 83.6-108.5%. Compared to liquid-liquid extraction methods, the Cis glass microcolumns give comparable results, lessen solvent costs, and are less time-consuming.

One hundred samples of dried fruits (20 dried raisins, 20 walnuts, 20 peanuts, 20 dried figs and 20 pistachios) and 20 samples of rice purchased from retail shops in the Rabat and Salé area in Morocco were analysed for ochratoxin A (OTA) by immunoaffinity clean-up (IAC) and liquid chromatography (LC) with fluorescence detection. The limit of quantification (LOQ) (S/N = 10:1) of OTA was 0.02 ng g(-1) in rice, 0.03 ng g(-1) in pistachio, peanut and walnut, and 0.03 ng g(-1) in dried raisins and dried figs. The incidences of occurrence of OTA in dried raisins, walnuts, peanuts, dried figs and rice were 30, 35, 25, 65 and 90%, respectively. Analytical results showed that pistachio samples contained no detectable OTA, but concentrations ranged from 0.02 +/- 0.01 to 32.4 +/- 2.10 ng g(-1) in rice, from 0.10 +/- 0.05 to 2.36 +/- 0.75 in peanut, from 0.03 +/- 0.01 to 1.42 +/- 0.45 in dried figs, from 0.05 +/- 0.02 to 4.95 +/- 0.02 in dried raisins, and from 0.04 +/- 0.01 to 0.23 +/- 0.05 in walnuts. The results also showed that 15% of the total number of rice samples analysed exceeded the 2002 regulatory limit set by European Union regulations for cereals. This is the first report on the occurrence of OTA in dried fruits and rice available in Morocco.

Washing with aqueous solutions of citric acid, ethanol, glycerol, hydrogen peroxide, potassium permanganate, sodium metabisulfite, sodium laurylsulfate (SLS), sodium hypochlorite, and urea is evaluated for pesticide residue reduction in nectarines and compared with simple tap water washing. Residues of pesticides commonly utilized in nectarines (chlorpyrifos, fenarimol, iprodione, malathion, methidathion, myclobutanil, parathion and pirimicarb) are extracted with ethyl acetate and anhydrous sodium sulfate, extract is concentred and analyzed by GC with nitrogen-phosphorus detection. The formation of possible toxic by-products (chlorpyrifos oxon, malaoxon, methidaoxon and paraoxon methyl) is studied by GC-MS. No toxic by-products are identified in the extracts of the washed samples for the washing-time and concentrations studied, but high levels of sodium hypochlorite, hydrogen peroxide and potassium permanganate form oxons from the organophosphorus pesticides. Ethanol, glycerol and SLS solutions removed near the 50% of the pesticide residues. The other solutions were not more effective than tap water washing. The amount of pesticide removed by washings is related to its water solubility and octanol-water partition coefficient.

Aflatoxin B1 (AFB1), B2 (AFB2), G1 (AFG1) and G2 (AFG2) were extracted by matrix solid-phase dispersion with C18 silica and acetonitrile as the eluting solvent, analysed by liquid chromatography with fluorescence detection and confirmed by liquid chromatography with mass spectrometry using an electrospray interface in 58 samples grouped as cereals, dried fruits, herbs and spices, pulses, snacks, and nuts and nut products collected from local markets and supermarkets in Valencia, Spain. All samples analysed by the proposed method were previously studied with an enzyme-linked immunosorbent assay as a screening protocol for the fast detection of mycotoxins. The samples containing residues (3/58) were hazelnut (0.42 and 0.52 microg kg(-1) for AFB1 and AFG1, respectively), nut cocktail (0.29 and 0.47 microg kg(-1) for AFB1 and AFG1, respectively) and pinhol (0.30 microg kg(-1) for AFG1). Such values were below the legislated maximum residue levels for the European Union.