Israel S. Ibarra

Magnetic solid phase extraction based on phenyl silica adsorbent for the determination of tetracyclines in milk samples by capillary electrophoresis

A magnetic solid phase extraction method coupled to capillary electrophoresis is proposed for the determination of tetracycline, oxytetracycline, chlortetracycline and doxycycline in milk samples. Five different magnetic phenyl silica adsorbents covered with magnetite were synthesized by varying the molar ratio of phenyltrimethylsilane and tetramethylorthosilicate; these adsorbents were evaluated in terms of their pH and degree of hydrophobicity for tetracycline retention. The optimal, selected combination of conditions was a pH of 10.0 and a magnetic sorbent ratio of 4:1; under these conditions, the retention capacity ranged from 99.7% to 101.2% for the four tetracyclines analyzed. The elution conditions and initial sample volume of the proposed extraction method were also optimized, and the best results were obtained with 1×10(-3) M acetic acid in methanol as eluent and a 200 ml of sample volume. Under optimal conditions, average recoveries ranged from 94.2% to 99.8% and the limits of detection ranged from 2 to 9 μg l(-1) for the four tetracyclines. After the proposed method was optimized and validated, 25 milk samples of different brands were analyzed, oxytetracycline residues were detected in five samples, in concentrations ranging from 98 to 213 μg l(-1). Subsequent analysis of positive samples by SPE-CE and magnetic solid phase extraction-HPLC revealed than no significant differences were found from results obtained by the proposed methodology. Thus, the developed magnetic extraction is a robust pre-concentration technique that can be coupled to other analytical methods for the quantitative determination of tetracyclines.

Magnetic solid phase extraction followed by high-performance liquid chromatography for the determination of sulphonamides in milk samples.

A simple and effective method based on magnetic solid-phase extraction combined with high performance liquid chromatography was used for the determination of nine sulphonamides in milk samples. The extraction and cleanup via silica-based magnetic adsorbent dispersion in milk samples followed by the magnetic isolation and desorption of the analytes using NaOH-methanol. Three different magnetic phenyl silica adsorbents were synthesized by varying the molar ratio of phenyltrimethylsilane and tetramethylorthosilicate; these adsorbents were evaluated for sulphonamides retention in terms of their pH and degree of hydrophobicity. The optimal conditions were a pH of 6.0 and a magnetic:sorbent ratio of 2:1. Under optimal conditions, limits of detection ranging from 7 to 14 μg L(-1) were obtained. The method was validated according with the European Commision Decision 2002/657/EC. The proposed method was applied to analyse sulphonamides in 27 milk samples of different brands. Thirteen samples tested were positive for the presence of sulphonamides.

Determination of quinolones in milk samples using a combination of magnetic solid-phase extraction and capillary electrophoresis

A magnetic solid‐phase extraction (MSPE) method combined with capillary electrophoresis for the simultaneous determination of seven quinolones (QNs) (danofloxacin, ciprofloxacin, marbofloxacin, enrofloxacin, difloxacin, oxolinic acid, and flumequine), using (S)‐(+)‐6‐methoxy‐α‐methyl‐2‐naphthaleneacetic acid as internal standard, in milk samples was developed. The variables involved in the preconcentration magnetic procedure were: the composition of the magnetic support composition, the sample pH, and the weight of magnetic adsorbent used. The variables were optimized using a simplex‐lattice design. Different magnetite covered with octyl‐phenyl silica adsorbents were synthesized by varying the molar ratio of phenyltrimethylsilane and octyltrimethoxysilane; the solids were evaluated for QN preconcentration. Under optimal conditions, a linear range was obtained from 27 to 1000 μg L−1 with limits of detection ranging from 9 to 12 μg L−1 for the seven QNs. The absolute recoveries of the seven QNs at three different spiked levels (40, 150, and 400 μg L−1) ranged from 74% to 98% with a relative standard deviation less than 10% in all cases. The proposed method was applied to analyze 20 whole milk samples of different brands. All samples were positive for the presence of QN residues; in some cases, extract dilution was required. The concentrations found are in the range from 31.1 to 5047.3 μg L−1. Marbofloxacin was the most frequently found. The method proposed offers advantages in terms of simplicity, sensitivity, efficiency, cost, and analysis time making it an alternative for the analysis of QNs in whole milk samples.

Magnetic Solid Phase Extraction Applied to Food Analysis

Magnetic solid phase extraction has been used as pretreatment technique for the analysis of several compounds because of its advantages when it is compared with classic methods. This methodology is based on the use of magnetic solids as adsorbents for preconcentration of different analytes from complex matrices. Magnetic solid phase extraction minimizes the use of additional steps such as precipitation, centrifugation, and filtration which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique which were applied in food analysis.

Magnetic solid phase extraction based on fullerene and activated carbon adsorbents for determination of azo dyes in water samples by capillary electrophoresis

A magnetic solid phase extraction method coupled to capillary electrophoresis for the simultaneous determination of three azo dyes (sunset yellow, allura red and tartrazine) in wastewater samples was proposed. The method employs the dispersion of magnetic adsorbents in the sample. Variables involved in the retention–elution procedures were optimized using a simplex centroid design. The optimal conditions were: an adsorbent composition of magnetite–activated carbon–fullerene (10 : 0.59 : 0.41), a sample pH of 4.0, and a sample volume (μl) : weight of adsorbent (mg) ratio of 0.01. Under optimal conditions, a linear range was obtained from 3.0–40.0 mg l−1 with limits of detection ranging from 1.0–2.0 mg l−1. The average recoveries of each dye at two spiked levels (10 and 25 mg l−1) ranged from 95–106% with relative standard deviations of less than 10% in all cases. The proposed method was applied to analyze wastewater samples from different locations. Two samples gave positive responses to the presence of tartrazine residues. The method proposed offers advantages in terms of simplicity, sensitivity, high efficiency, low cost, and short analysis time, making it an alternative for the analysis of azo dyes in water samples and other complex matrices.

Sequential Injection Magneto Chromatography Determination of Non-Steroidal Anti-Inflammatory Drugs in Pharmaceutical Formulations

A magnetic separation method based on the use of magnetic silica as the stationary phase in sequential injection chromatography was used for simultaneous determination of nonsteroidal anti-inflammatory drugs (acetaminophen, naproxen, diclofenac, and ibuprofen) in tablets. The method is based on a thin layer paramagnetic stationary phase retained on the inner wall of a mini-column through the action of an external magnetic field. The influence of the variables involved was evaluated and the optimal conditions were found to be: a methyl-silica magnetic adsorbent was used as the stationary phase, the mobile phase was methanol-water (60:40, v/v), pH 2.5 adjusted with 98% phosphoric acid, a flow rate 0.60 ml min−1, and UV detection at 225 nm. Under these conditions, the linear range of the calibration curve ranged from 3–6 mg L−1 to 100 mg L−1 with limits of detection ranging between 1 to 2 mg L−1. The proposed method was validated by comparing the results obtained against those provided by high performance liquid chromatography; no significant differences were seen.

Solid-Phase Extraction and Large-Volume Sample Stacking-Capillary Electrophoresis for Determination of Tetracycline Residues in Milk

Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE) was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200 µg·L−1, with limits of detection ranging from 18.6 to 23.8 µg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation) in all cases. The enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE). This method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. The proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 µg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices.

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis.

Effect of Packaging Systems on the Inactivation of Microbiological Agents

Abstract The potential microbial contamination by spoilage and pathogenic microorganisms is a major concern, because it reduces the shelf life of foods and increases the risk of foodborne diseases. Antimicrobial packaging is playing an important role in the inhibition of targeted bacterial growth on food, while improving food safety and prolonging shelf life, without sacrificing the quality. Traditionally, non-biodegradable synthetic polymers have been employed for antimicrobial food packaging (AFP). However, nowadays, in some countries, there is a great interest in avoiding food wastage and reducing the use of plastics, as well as the reutilization of waste originated during food production. Consequently, commercial applications of antimicrobial packaging are expected to grow in the next few years. This is especially true for applications that employ active compounds derived from natural resources and biodegradable packaging materials as carrier polymers. This chapter provides a broad overview of the antimicrobials and matrixes employed for AFP, their advantages, and disadvantages, as well as their future trends.

Development of Cellulose Acetate Microcapsules with Cyanex 923 for Phenol Removal from Aqueous Media

Microcapsules of cellulose acetate with Cyanex 923 were prepared and used in this study for phenol removal from water and synthetic textile wastewater. The influence of several factors on the microcapsules extraction efficiency was studied, as well as characterization and phenol adsorption isotherm. Microcapsules characterization demonstrated the extractant reagent encapsulation, while in a batch mode procedure, good adsorption of phenol (ca. 5.5 × 10−3 mol Kg−1) has been reached. A slight decrease in phenol extraction percentage was obtained when synthetic textile wastewater was used (ca. 4.955 × 10−3 mol Kg−1), although a decrease in color was observed due to dye microcapsule extraction. Results indicate that this method is a promising alternative to conventional phenol removal technologies for aqueous samples of low phenol concentrations or in textile effluents.