Pulse Duration and Efficiency of Soft Cellular Tissue Disintegration by Pulsed Electric Fields

The effect of pulse duration on efficiency of disintegration of apple tissue by pulsed electric fields (PEF) was studied. The samples (26-mm diameter, 10-mm height) were treated by PEF at electric field strength E between 100 and 400 V/cm, pulse duration t _i of 10, 100, 1,000 μs, inter-pulse duration Δt of 100 μs and different number of pulses n. Both the degree and the time evolution of tissue damage were quantified by electrical conductivity disintegration index Z and characteristic damage time τ, respectively. The samples exposed to the same PEF treatment time nt _i showed noticeably higher disintegration efficiency for larger pulse duration. The synergism of PEF and thermal treatment with temperature T (20–50 °C) was demonstrated. The Arrhenius dependence of τ(T) for PEF treatment at E = 100 V/cm gave the decreasing activation energy W as a function of t _i, (Q ≈ 164 kJ/mol at t _i = 10 μs, Q ≈ 109 kJ/mol at t _i = 100 μs and Q ≈ 66 kJ/mol at t _i = 1,000 μs). Textural relaxation data supported the higher damage efficiency for longer pulse duration.     

Simultaneous Determination of 69 Pesticide Residues in Coffee by Gas Chromatography?CMass Spectrometry

A method using gel permeation chromatography (GPC) combined with solid-phase extraction (SPE) cleanup followed by gas chromatography–mass spectrometry (GC-MS) has been established for quantitative determination of 69 pesticide residues in coffee. Based on an appraisal of the characteristics of GC-MS, validation experiments were conducted for 69 pesticides. In the method, 2.0 g samples were mixed with 5 ml water and 1 g sodium chloride and extracted with 5 ml of ethyl acetate by blender homogenization, centrifugation, and filtration. Evaporation was conducted and the sample was injected into a 250 mm × 10 mm S-X3 GPC column, with ethyl acetate–n-hexane (1:2 v/v) as the mobile phase at a flow rate of 3 ml/min. The 4–15 min fraction was collected for the SPE cleanup, which was Envi-Carb SPE cartridge coupled with NH₂-LC SPE cartridge with acetone–ethyl acetate (2:5 v/v) as the eluted solvent. The eluents were collected and then evaporated to dryness, which was redissolved in 0.5 ml ethyl acetate for GC-MS analysis. For the 69 pesticides determined by GC-MS, the portions collected from GPC were concentrated to 0.5 ml and exchanged with 5 ml n-hexane. In the linear range of each pesticide, the correlation coefficient was R ² ≥ 0.99. At the low, medium, and high fortification levels of 0.05–1.0 mg/kg, recoveries fell within 60–120%. The relative standard deviation was between 1.3% and 22.3% for all 69 pesticides. The limits of detection for the method were 10 μg/kg to 150 μg/kg, depending on each pesticide.     

Liquid Chromatographic Determination of Resveratrol and Piceid Isomers in Honey

In this work, a liquid chromatography method with diode array and fluorescence detection and electrospray ionization mass spectrometry (LC-DAD-FLD and LC-ESI-MS) has been developed for the determination of residues of resveratrol in all its forms (free isomers and glycosylates) in honey. This procedure involves a solid-phase extraction on polymeric cartridges for the isolation of trans/cis-isomers of resveratrol and piceid from diluted honey samples. Chromatographic separation of the analytes was performed in isocratic mode on a C₁₈ column (150 mm × 4.6 mm i.d., 5 μm) operated at 30 °C. The mobile phase consisted of a mixture of water with 1% formic acid and acetonitrile (75/25, v/v), and the flow rate was set at 1.0 mL/min. Average analyte recoveries were from 71% to 113% in replica sets of fortified honey samples. The detection limits when using LC-DAD-FLD were between 40 and 120 μg/kg, meanwhile for LC-ESI-MS were between 1.4 and 14.6 μg/kg. The proposed method was applied to the analysis of honey samples collected from treated beehives in experimental apiaries after a preliminary field trial, and they were not found any residues over the detection limits of the studied compounds.     

Determination of Rosmarinic Acid by High-Performance Liquid Chromatography and Its Application to Certain Salvia Species and Rosemary

This study describes a method development for the determination of rosmarinic acid (RA) by using a gradient high-performance liquid chromatography (HPLC) and its application to certain plant materials. The analysis was performed by utilizing a two solvents system [A: methanol/water/formic acid (10:88:2; v:v:v); B: methanol/water/formic acid (90:8:2; v:v:v)] on a reverse-phase column. The flow rate and injection volume were 1 ml min⁻¹ and 10 μl, respectively. Signals were detected at 280 nm. In addition, an internal standard (IS) technique was applied for the analysis of RA to increase precision, and propylparaben was employed for this purpose. The repeatability results as RSD% were 1.66, 1.17 and 1.26 for intra-day and 1.38 was for inter-day with the employment of (3.67 × 10⁻⁵ M) RA. A limit of linearity (LOL) was observed in a wide (1.13 × 10⁻⁵–5.65 × 10⁻⁴ M) concentration range. Linearity parameters were also examined in the range of 5.95 × 10⁻⁶–7.14 × 10⁻⁵ M RA, and very good correlation was observed. The limit of detection (LOD) and limit of quantification (LOQ) (for inter-day) were 1.60 × 10⁻⁶ M (signal/noise [S/N] = 3.3) and 4.80 × 10⁻⁶ M (S/N = 10), respectively. The method was applied to the extracts of certain Lamiaceae plants (Salvia candidissima Vahl. subsp. candidissima, S. sclarea L., S. verticillata L. subsp. verticillata and R. officinalis L.), and reasonable results were obtained.     

Structural Relaxation of Salmon Gelatin Films in the Glassy State

Mechanical relaxation of glassy carbohydrates has been reported extensively in the literature; however, little work is available on protein-based systems. This study deals with the structural relaxation of salmon (Salmo salar) gelatin in the glassy state. Skin gelatin was obtained by an acid–alkaline extraction method. Molecular weight (M _w) was determined by capillary viscometry. Films prepared by casting (7% w/v) were equilibrated to a moisture content of ~18.4% (db). The glass transition temperature (T _g) and enthalpic relaxation were determined by differential scanning calorimetry (DSC). Mechanical properties were assessed using a texture analyzer at constant temperature and moisture content. DSC showed a T _g ~34°C, and the selected storage temperature (T _a ) was 29°C (T _g − T _a = 5°C). The films were aged for 0, 4, 8, 16, and 40 h. Viscometry produced values of M _w ~90.2 kDa. The stress relaxation was modeled by the Kohlrausch–Wlliams–Watts (KWW) equation, reporting an increase in relaxation time (τ ₀) as the ageing time increased (τ ₀ ~6.41E + 03 s for 0 h; τ ₀ ~9.01E + 05 s for 40 h). β parameter was smaller for the aged films, indicating a spread of relaxation times. The derivative of KWW equation (dφ/dt) indicated a more rapid relaxation in a fresh sample compared with aged films. DSC showed an excess in enthalpy (ΔH) on the aged samples due to the non-equilibrium state of the matrix. ΔH increased with ageing time with values of ΔH ~2.42 J/g for the films aged for 40 h. This work demonstrated molecular relaxation process of gelatin in the glassy state, which must be taken into account if this material is used as a structure forming matrix.     

A Simple and Fast Method for Determination of Phosphorus in Fish Diets and Faeces Used in Animal Nutritional Studies

The optimization and validation of a simple and fast analytical method for the determination of phosphorus in fish diets and faeces used in animal nutrition studies are shown in this paper, starting with the validation of a pre-optimized digestion procedure for biological samples, choice of the best chemical modifier and the minimal sample amounts. The digestion procedure consisted of an acid dissolution of a minimal of 100 mg of dry sample in a domestic microwave system using Parr Teflon bombs at high pressure. The P levels were determined by atomic absorption spectrometry with electrothermal atomisation, using an absorbance of 213.6 nm, a slit width of 1.0 nm, a current lamp of 20 mA and a deuterium lamp for background correction. Different furnace temperature programmes were used, and a final temperature programme was optimized. The optimization stages suggested the use of a 1,000 μg/ml La solution as chemical modifier and 1,600 and 2,700 °C as, respectively, the best pyrolysis and atomisation temperatures. The optimized analytical method was applied to different types of fish diets and faeces, and the percentages of recovery of P in spiked samples were, respectively, 94 ± 11% (n = 3) and 100 ± 12% (n = 3). The detection limit was 0.15 mg P/g of dry sample. The optimized methodology is simpler, faster and has less sample mass consumption than normally used colorimetric methods.     

Phenolic Content and Antioxidant Activity of Moscatel Dessert Wines from the Setúbal Region in Portugal

Moscatel wines from Setúbal were analyzed for their total phenolic (mean value 1,243 mg gallic acid equivalents/L), and total flavonoid (mean value 248 mg catechin/L) composition by spectrophotometric and chromatographic methods were used to quantify phenolic compounds as benzoic acids, cinnamic acids, stilbens, and some flavonoids. Antioxidant activity of the wines was evaluated by 1,1-diphenyl-2-picrylhydrazyl (DPPH; mean value 70.7% inhibition), ferric reducing antioxidant power (FRAP; mean value 3,098 mg of Trolox equivalents/L) and oxygen radical absorbance capacity (ORAC; mean value 10,724 μmol/L) assays. Results were analyzed using principal component analysis which allowed samples to be grouped in terms of both winemaking producer and vintage. By plotting correlation loadings, it was possible to understand which variables were responsible for sample distribution. The correlation between results obtained for variables show that, in general, total flavonoid content is a better estimation of antioxidant activity in Moscatel samples (r _{ORAC/flavonoids} = 0.832, r _{FRAP/flavonoids} = 0.677) than total phenolic content (r _{ORAC/phenolics} = 0.680, r _{FRAP/phenolics} = 0.372). No major correlations were detected for DPPH assay results (r _{DPPH/flavonoids} = 0.283, r _{DPPH/phenolics} = 0.271). Chromatographic profiles showed important differences among Moscatel wines. Gallic acid contents and results of antioxidant activity tests were strongly correlated (r values in the range 0.74–0.92). Correlations of the results obtained for antioxidant activity tests with contents of other phenolic compounds such as ethyl caffeate, ethyl gallate, caffeic acid, protocatechuic acid, and t-caftaric acid depend on sample and type of test employed. Presented at the “AOAC Europe section international workshop: Enforcement of European Legislation on Food and Water: Analytical and Toxicological Aspects”, in Lisbon, April 2008, and published in abstract form.     

GFAAS Determination of Zinc in Fish Feed and Feces Using Slurry Sampling

This paper presents a simple, fast, and sensitive method to determine zinc in samples of feces and fish feed by electrothermal atomic absorption spectrometry through the direct introduction of slurries of the samples into the spectrometer’s graphite tube. The procedure is based on the injection of 10 μL of an acidified aqueous solution containing 0.50% w/v of feces or feed and 0.50% v/v HNO₃ into graphite tube. The limits of detection and quantification calculated for 20 readings of the blank of the standard slurries (0.50% w/v of feces or feed devoid of zinc) were 0.04 and 0.13 μg L⁻¹ for the standard feces slurries and 0.05 and 0.17 μg L⁻¹ for the standard feed slurries. The proposed method was applied in studies of digestibility of zinc in different fish feeds, and their results proved compatible with that obtained from samples mineralized by acid digestion using microwave oven.     

A Rapid Spectrophotometric Method for Trace Determination of Zinc

A simple, sensitive, and highly selective method is proposed for the determination of zinc(II) using a bis-azo dye, 2,6-bis(1-hydroxy-2-naphthylazo)pyridine as spectrophotometric reagent. At pH 7.8, in 50% (v/v) ethanol–water medium, the complex is found to obey Beer’s law up to 1.3 mg/L with an optimum concentration range between 0.19 and 1.0 mg/L. Sandell’s sensitivity of the color reaction was calculated to be 0.0011 μg cm⁻² with molar absorptivity of 6.0 × 10⁴ L mol⁻¹ cm⁻¹ at 560 nm. The optimum conditions for the determination of Zn(II) with the reagent were ascertained. The complexation at different pH was studied in water–ethanol medium. The composition of the complex is 1:2. The action of some interfering ions was verified, and the developed method applied successfully for the estimation of zinc levels in food and milk samples, and the results were then compared with those obtained by using AAS.     

Production and Application of Xylanase from Penicillium sp. Utilizing Coffee By-products

The lignocellulosic coffee by-products such as coffee pulp, coffee cherry husk, silver skin, and spent coffee were evaluated for their efficacy as a sole carbon sources for the production of xylanase in solid-state fermentation using Penicillium sp. CFR 303. Among the residues, coffee cherry husk was observed to produce maximum xylanase activity of 9,475 U/g. The process parameters such as moisture (50%), pH (5.0), temperature (30 °C), particle size (1.5 mm), inoculum size (20%), fermentation time (5 days), carbon source (xylose), and nitrogen source (peptone) were optimized and the enzyme activity was in the range of 19,560–20,388 U/g. The enzyme production was further improved to 23,494 U/g with steam as a pre-treatment. The extracellular xylanase from the fungal source was purified to homogeneity from culture supernatant by ammonium sulfate fractionation, DE32-cellulose with a recovery yield of 25.5%. It appeared as a single band on SDS-PAGE gel with a molecular mass of approximately 27 kDa. It had optimum parameters of 50 °C temperature, pH 5.0, K _m 5.6 mg/mL, and V _max 925 μmol mg⁻¹ min⁻¹ with brichwood xylan as a substrate. The crude enzyme hydrolysed lignocellulosic substrate as well as industrial pulp. Production of xylanase utilizing coffee by-products constitutes a renewable resource and is reported for the first time.     

Analysis of Flavonoids in <Emphasis Type="Italic">Portulaca oleracea</Emphasis> L. by UV–Vis Spectrophotometry with Comparative Study on Different Extraction Technologies

Portulaca oleracea L. is a traditional edible and medicinal plant in China. Flavonoids are one of the main active ingredients of this plant. Five extraction technologies of flavonoids from P. oleracea L. were investigated and compared, including microwave-assisted extraction, ultrasonic extraction, reflux extraction, Soxhlet extraction, and marinated extraction. The results showed that microwave-assisted extraction was most suitable for the extraction of flavonoids from P. oleracea L. because of its high effect and short extraction time. The found optimum extraction conditions were that the ethanol concentration was 70% (v/v), solid–liquid ratio was 1:50, extracting temperature was 50 °C and irradiation time was 9 min. Quantification was performed by means of UV–Vis spectrophotometry with chromogenic system of NaNO₂–Al (NO₃)₃–NaOH. Under the optimum conditions, the calibration curve for the analyte was linear with the correlation coefficients greater than 0.9999. The average recovery was 102.6%, and its RSD was 1.13%(n = 5). Eight types of P. oleracea L. according to different habits were investigated. The total content of flavonoids was 7.16, 7.10, 9.38, 6.82, 6.78, 11.36, 5.12, and 1.76 mg g⁻¹, respectively.     

Concentrations of cadmium and lead in different types of milk

 Concentrations of Pb and Cd were determined in samples of human, raw and pasteurized cow's and goat's milk and powdered infant formula. The following mean Cd concentrations (and ranges) were recorded: in human milk, 2.70 μg/l (0.6–11.3, n=55); in raw cow's milk, 4.88 μg/l (0.7–23.1, n=47); in pasteurized cow's milk, 4.30 μg/l (3.4–5.9, n=6); in goat's milk, 7.81 μg/l (1.0–18.4, n=38); and in powdered, infant formula, 3.81 μg/l (3.4–4.1, n=5). The concentrations (and ranges) of Pb were: in human milk, 8.34 μg/l (0.1–32.3, n=55); in raw cow's milk, 14.82 μg/l (1.3–39.1, n=28); in pasteurized cow's milk, 10.25 μg/l (6.9–19.6, n=6); in goat's milk, 11.86 μg/l (0.4–38.5, n=36); and in powdered, infant formula, 8.30 μg/l (5.1–10.6, n=5). Our data were within the normal ranges for each kind of milk. The Cd and Pb concentrations in goat's milk were significantly higher than the concentrations observed in the other milks, whereas human milk and powdered infant formula presented the lowest Cd and Pb concentrations. A considerable decrease in the concentration of Cd with the stage of lactation was observed. The concentrations of Cd and Pb in human, cow's and goat's milk also varied according to the time of year. The concentrations of Pb and Cd in the different milks did not present any risk to human health (infants or adults). Received: 26 May 1998     

Optimization of Conditions for Enzymatic Production of ACE Inhibitory Peptides from Collagen

Enzymatic condition for producing angiotensin I-converting enzyme (ACE) inhibitory peptides from collagen was optimized with the aid of response surface methodology, which also derived a statistical model for experimental validation. The results showed that the optimal condition for the hydrolysis by pepsin was at pH 2, temperature 37 °C, and in enzyme to substrate ratio (E/S) of 2 when 8.23% collagen (w/v) and 3.82 h of hydrolysis time were applied. Through the single-enzyme hydrolysis, the ACE inhibitory activity could reach an average of 78.06%. In contrast, when a combination of pepsin and trypsin was used for a multiple-proteases hydrolysis, the ACE inhibitory activity could be significantly improved to an average of 88.25%. Furthermore, the IC₅₀ (μg/mL) value of the enzyme combination by pepsin and trypsin (141.64 ± 22.11) was significantly lower than that of the combinations of pepsin and papain (438.59 ± 84.37) or pepsin and protease M (336.76 ± 87.88; p<0.05). Our results have shown that collagen can be used for enzyme-mediated production of ACE inhibitory peptides.     

Storage Properties of Low Fat Fish and Rice Flour Coextrudates

In the present study, response surface method (RSM) and genetic algorithm (GA) were used to study the effects of process variables like screw speed, rpm (x ₁), L/D ratio (x ₂), barrel temperature (°C; x ₃), and feed mix moisture content (%; x ₄), on flow rate of biomass during single-screw extrusion cooking. A second-order regression equation was developed for flow rate in terms of the process variables. The significance of the process variables based on Pareto chart indicated that screw speed and feed mix moisture content had the most influence followed by L/D ratio and barrel temperature on the flow rate. RSM analysis indicated that a screw speed > 80 rpm, L/D ratio > 12, barrel temperature > 80 °C, and feed mix moisture content > 20% resulted in maximum flow rate. Increase in screw speed and L/D ratio increased the drag flow and also the path of traverse of the feed mix inside the extruder resulting in more shear. The presence of lipids of about 35% in the biomass feed mix might have induced a lubrication effect and has significantly influenced the flow rate. The second-order regression equations were further used as the objective function for optimization using genetic algorithm. A population of 100 and iterations of 100 have successfully led to convergence the optimum. The maximum and minimum flow rates obtained using GA were 13.19 × 10⁻⁷ m³/s (x ₁ = 139.08 rpm, x ₂ = 15.90, x ₃ = 99.56 °C, and x ₄ = 59.72%) and 0.53 × 10⁻⁷ m³/s (x ₁ = 59.65 rpm, x ₂ = 11.93, x ₃ = 68.98 °C, and x ₄ = 20.04%).     

Listeria innocua Multi-target Inactivation by Thermo-sonication and Vanillin

Hurdle technology combining an emerging preservation technique such as low-frequency ultrasound is an alternative for processing juices that are susceptible to suffer a loss of quality due to traditional heat treatments. Predictive microbiology allows evaluation of the effectiveness of preservation techniques and its combinations in order to enhance both food quality and safety. Listeria innocua inactivation by thermo-sonication along with vanillin was investigated. Fermi model (R ² _adj= 0.970 ± 0.02) and surface response methodology (p < 0.05) were utilized in order to evaluate the survival of L. innocua to a multi-target treatment and to predict the interactions of studied techniques, high-intensity/low-frequency ultrasound (20 kHz/400 W) at selected wave amplitudes (60, 75, or 90 μm), temperature (40, 50, or 60 °C), and vanillin (200, 350, or 500 mg/kg). A combination of ultrasound, vanillin, and temperature enhanced L. innocua inactivation as described by Fermi parameters a and t _c, which decreased as the studied effects increased. A multi-target inactivation effect was observed for a temperature range of 45–55 °C.     

Evaluation and Quantification of Heat Treatments Applied to Food Preserves

The quantitative study of heat treatments for sterilisation uses the Bigelow model to calculate the sterilising value (F). Calculation of F requires the previous determination of parameters D (decimal reduction time at experimental temperature) and Z (thermal-death time parameter), obtained from the thermal-death kinetics. Herein we compare two different methods, namely the Bigelow model and a predictive-type statistical method, to calculate the sterilisation effect against Bacillus coagulans spores when heat was applied to runner bean preserves (variety: Helda). Samples were subjected to various autoclave treatments at working temperatures (T _ai) of 105, 107, 110, and 115°C for periods from 3 to 35 min. The microorganism used was B. coagulans. Sterilisation achieved by these autoclave treatments was determined by using the equation based on the Bigelow model (n _probe = F ^z _Ti/D _Ti) where n is the fractional concentration of colony-forming units (or some quality factor), F ^z _Ti is F at temperature T _i, and D _Ti is D at temperature T _i. The Bigelow model can be used to obtain Z (thermal-death time parameter), which is needed to calculate the traditional sterilisation factor F, but not to determine the reduction factor n for the heat treatments, particularly when microbial indicators with low decimal reduction times (D) are studied. The thermokinetic parameters for B. coagulans in runner bean solution resulted to be Z = 10.64°C and D ₁₂₁ = 0.0264 min (Af = 1.04). Treatment at 115°C for 20 min resulted in the most efficient sterilisation effect for B. coagulans.     

Total Mercury, Inorganic Mercury and Methyl Mercury Determination in Red Wine

This study deals with the development of a method for total Hg, inorganic Hg and methylmercury (MeHg) determination in red wine by using flow injection-cold vapour generation–inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS) and gas chromatography-ICP-MS (GC-ICP-MS). For Hg speciation analysis, a derivatization step was carried out using a 1% (m/v) sodium tetraphenylborate (NaBPh₄) solution, followed by extraction of Hg species and their quantification by GC-ICP-MS. The main parameters evaluated were the make-up gas flow rate, volume of the NaBPh₄ solution, time for derivatization reaction/analyte extraction and solvent used for Hg species extraction. Accuracy was evaluated by analyte recovery, whereas recoveries ranged from 99% to 104% for Hg(II) and MeHg. The limits of detection (LODs) for Hg(II) and MeHg were 0.77 and 0.80 μg L⁻¹, respectively. Wine from Argentina, Brazil, Chile and Uruguay were analysed. The wine samples were also acid digested for total Hg determination by FI-CVG-ICP-MS. The LOD of the method used for total Hg determination was 0.01 μg L⁻¹. The concentrations of Hg species in red wine measured by GC-ICP-MS were lower than the respective LODs. Only total Hg was detected in the analysed samples, where the highest concentration of Hg found was 0.55 ± 0.02 μg L⁻¹.     

Thermal Transition Properties of Spaghetti Measured by Differential Scanning Calorimetry (DSC) and Thermal Mechanical Compression Test (TMCT)

Glass transition temperature (T _g) of spaghetti sample was measured by thermal and rheological methods as a function of water content from 0 to 70 kg/100 kg spaghetti. In the cases of sample containing un-freezable water (i.e., amount of water which did not form ice even at very low temperature), calorimetric measurements performed by differential scanning calorimetry showed that the T _g values decreased from 142.8 to 42.7 °C when water content increased from 0 to 13.95 kg/100 kg spaghetti, respectively. Glass transition temperature increased with the increase of heating rate (2–50 °C/min) and reached to a nearly constant value above 30 °C/min. Thermal mechanical compression test showed relatively lower T _g values compared to the DSC values at low moisture contents, whereas at high moisture content T _g showed higher values. In the cases of samples containing freezable water (27–70 kg/100 kg spaghetti), glass transition shifts were merged with the ice melting endotherm. The freezing point, measured from the endothermic peak, decreased with the decrease of water content. In the state diagram, maximal freeze-concentration condition was determined as X_\texts￠ X_{\text{s}}^\prime =0.81 kg/kg spaghetti from the intersection of the extended freezing curve and a horizontal line passing thru T_\textm￠ T_{\text{m}}^\prime  = −10.3 °C.     

Optimization of supercritical CO2 extraction of phytosterol-enriched oil from Kalahari melon seeds

Supercritical carbon dioxide (SC-CO₂) extraction of oil from Kalahari melon seeds was investigated in this study. Response surface methodology was applied to model and optimize the extraction, namely pressure (200–400 bar), temperature (40–80 °C), and supercritical fluid flow rate (10–20 mL/min). Well-fitting models were successfully established for oil recovery (R ² = 0.9672) and phytosterol concentration (milligrams per 100 g; R ² = 0.8150) through multiple linear regressions with backward elimination. The effect of supercritical fluid flow rate was the most significant (P < 0.05) factor that affected oil recovery but this factor had no significant (P > 0.05) effect on phytosterol concentration. The optimal processing conditions for oil recovery and phytosterol concentration were pressure of 300 bar, temperature at 40 °C, and supercritical fluid flow rate of 12 mL/min. These optimal conditions yielded a 76.3% oil recovery and 836.5 mg/100 g of phytosterol concentration. The oil content in the Kalahari melon seeds as estimated by Soxhlet extraction was around 30.5/100 g. The phytosterol concentration in the oil extracted with SC-CO₂ extraction was 94% higher than that obtained with solvent extraction.     

Screening of Fluoroquinolone Residues in Caprine Milk Using a 5-kg Luminescence Photometer

Fluoroquinolone (FQ) residues in caprine milk were screened by terbium-sensitized luminescence (TSL). After extraction and cleanup using Oasis HLB columns, TSL was measured at λ _ex = 300 nm and λ _em = 546 nm using a 5-kg luminescence photometer. A common threshold was established at x _F50–3σ _F50, where x _F50 and σ _F50 were the mean and standard deviation, respectively, of TSL intensities of milk samples (n = 18) spiked with flumequine at 50 ng/g, its maximum residue limits (MRL) set by the European Union. Enrofloxacin, ciprofloxacin, and danofloxacin at their respective MRLs had higher TSL responses, so could be screened below their MRLs. Among 48 blind samples, each randomly spiked with one FQ at up to 200% of its MRL, 36 were screened correctly without false negative. This rapid protocol can reduce a sample pool to a small fraction for confirmation, hence improve throughput and save assay costs.