Determination of hippuric acid in human urine by ion chromatography with conductivity detection

A simple, rapid, precise and eco-friendly ion chromatography (IC) method for the determination of hippuric acid (HA) in human urine was proposed in this paper. The separation was carried out an anion exchange column with 2.0 mmol L^?1 Na₂CO₃ + 2.0 mmol L^?1 NaHCO₃ as mobile phase at the flow-rate 0.7 mL min^?1. A suppressed conductivity detector was used and the detection limit was 1.0 μg L^?1(S/N = 3) for hippuric acid. The analysis time for one run was 30 min under the optimized IC condition. The recovery of hippuric acid was 93.2–98.0% while the relative standard deviation (RSD) was 1.4–2.3% by seven measurements.     

Direct LC-ES-MS/MS determination of phthalates in physiological saline solutions

A method for determining a group of phthalic esters (PAEs) in physiological saline solutions has been developed. The PAEs studied were dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate and dibutyl phthalate. These groups of phthalates were determined by liquid chromatography–electrospray ionization-tandem mass spectrometry, working in positive ion mode. The compounds were separated by liquid chromatography working in gradient mode with acetonitrile–ultrapure water as a mobile phase. The separation was performed starting with 5% of acetonitrile and increasing to 75% in 5 min, followed by isocratic elution for 8 min. The method was precise (with relative standard deviation (RSD) from 1.0 to 6.8%) and sensitive, with LODs of 0.05, 0.38, 0.05 and 0.82 μg L^?1 for DMP, DEP, BBP and DBP, respectively. The proposed analytical method has been applied to determine these compounds in different physiological saline solutions commercialized in plastic bottles.     

Predictive modeling of biomass production by Spirulina platensis as function of nitrate and NaCl concentrations

Effects of nitrate (2.0, 2.5, and 3.0 g L^?1) and salt (0.5, 1.0, 1.5, 2.0 g L^?1) concentrations on biomass production by Spirulina platensis was examined in the Schlösser medium. The highest (p < 0.001) biomass yields and chlorophyll a content was observed at 2.5 g L^?1 nitrate and 1.5 g L^?1 NaCl as 3.495 g L^?1 and 29.92 mg L^?1, respectively. Increment rate of biomass production was especially found between 72 and 216 h. Modified Richards, Schnute, Logistic and Gompertz models was successfully predicted (r² > 0.96 and RSS ? 0.003) biomass production by S. platensis as function of nitrate and salt concentrations. Low residual sum of squares (RSS) and high regression coefficients (r²) indicated that used models were well fitted to the experiment data and it could be regarded as sufficient to describe biomass production of Spirulina sp. Biological variables i.e. production rate (μ) and lag time (λ) for S. platensis ranged 0.012–0.034 h^?1 and 2.43–5.85 h, respectively from biomass production were successfully predicted by modified Logistic model according to low RSS and F-testing value.     

Enhancing the value of nitrogen from rapeseed meal for microbial oil production

Rapeseed meal, a major byproduct of biodiesel production, has been used as a low-cost raw material for the production of a generic microbial feedstock through a consolidated bioconversion process. Various strategies were tested for the production of a novel fermentation medium, rich in free amino nitrogen (FAN): commercial enzymes (CEs) (2.7 mg g^?1 dry meal), liquid state fungal pre-treatment (LSF) using Aspergillus oryzae (4.6 mg g^?1), liquid state fungal pre-treatment followed by fungal autolysis (LSFA) (9.13 mg g^?1), liquid state pre-treatment using fungal enzymatic broth (EB) (2.1 mg g^?1), but the best strategy was a solid state fungal pre-treatment followed by fungal autolysis (34.5 mg g^?1).The bioavailability of the nitrogen sources in the novel medium was confirmed in fed-batch bioreactor studies, in which 82.3 g dry cell L^?1 of the oleaginous yeast Rhodosporidium toruloides Y4 was obtained with a lipid content of 48%. The dry cell weight obtained was higher than that obtained using conventional yeast extract, due to a higher total nitrogen content in the novel biomedium. The fatty acids obtained from the microbial oil were similar to those derived from rapeseed oil.     

A method for CP 47, 497 a synthetic non-traditional cannabinoid in human urine using liquid chromatography tandem mass spectrometry

A rapid method has been developed to analyse CP 47, 497 in human urine. Urine samples were diluted with water:acetonitrile (90:10, v/v) and sample aliquots were analysed by triple quadrupole tandem mass spectrometry with a runtime of 5 min. Multiple reaction monitoring (MRM) as survey scan was performed. The method was validated in urine, according to an in-house validation protocol based on the criteria defined in Commission Decision 2002/657/EC. Three MRM transitions were monitored. The decision limit (CCα) was 0.01 μg mL^?1 and for the detection capability a (CCβ) value of 0.02 μg mL^?1 was obtained. The measurement uncertainty of the method was 21%. Fortifying human urine samples (n = 18) in three separate assays, show the accuracy of the method to be between 95 and 96%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (0.1, 0.15 and 0.2 μg mL^?1) was less than 10% respectively. The method proved to be simple, robust and time efficient. To the best of our knowledge there are no LC–MS methods for the determination of CP 47, 497 with validation data in urine.     

Criteria to distinguish between natural situations and illegal use of boldenone,boldenone esters and boldione in cattle: 2. Direct measurement of 17β-boldenone sulpho-conjugate in calf urine by liquid chromatography–high resolution and tandem mass spectrometry

Boldenone is banned in the European Union (Directive 96/22/EC) as growth promoter for meat producing animals. Boldione (ADD), boldenone and boldenone esters (mainly the undecylenate form) are commercially available as anabolic preparations, either to the destination of human, horse or cattle. Since the late 90s, the natural occurrence of boldenone metabolites has been reported in cattle. According to EU regulation, the unambiguous demonstration of boldenone administration in bovine urine should be provided on the basis of boldenone identification in the corresponding conjugate fraction. An analytical method has been developed and validated according to current standards with main concern to the measurement of intact 17β-boldenone-sulphate. The analytical procedure included direct extraction–purification of target analyte on octadecylsilyl cartridges and direct detection of phase II metabolite by liquid chromatography (negative electrospray), tandem mass spectrometry (QqQ) or high resolution mass spectrometry (Orbitrap?). Decision limit (CCα) and detection capability (CCβ) were respectively 0.2 μg L^?1 and 0.4 μg L^?1 on triple quadrupole and 0.1 μg L^?1 and 0.2 μg L^?1 on hybrid system. The method was successfully applied to the analysis of incurred samples collected in different experiments. 17β-Boldenone-sulphate was measurable up to 36 h after oral administration of boldione, and 30 days after 17β-boldenone undecylenate intra-muscular injection. This conjugate form was never detected in non-treated animals, confirming its status of definitive candidate marker for boldenone administration in calf.     

Rapid confirmatory method for the determination of sixteen synthetic growth promoters and bisphenol A in bovine milk using dispersive solid-phase extraction and liquid chromatography–tandem mass spectrometry

A rapid liquid chromatographic–tandem mass spectrometric (LC–MS/MS) multi-residue method for the simultaneous quantitation and identification of sixteen synthetic growth promoters and bisphenol A in bovine milk has been developed and validated. Sample preparation was straightforward, efficient and economically advantageous. Milk was extracted with acetonitrile followed by phase separation with NaCl. After centrifugation, the extract was purified by dispersive solid-phase extraction with C18 sorbent material. The compounds were analysed by reversed-phase LC–MS/MS using both positive and negative ionization and operated in multiple reaction monitoring (MRM) mode, acquiring two diagnostic product ions from each of the chosen precursor ions for unambiguous confirmation. Total chromatographic run time was less than 10 min for each sample. The method was validated at a level of 1 μg L^?1. A wide variety of deuterated internal standards were used to improve method performance. The accuracy and precision of the method were satisfactory for all analytes. The confirmative quantitative liquid chromatographic tandem mass spectrometric (LC–MS/MS) method was validated according to Commission Decision 2002/657/EC. The decision limit (CCα) and the detection capability (CCβ) were found to be below the chosen validation level of 1 μg L^?1 for all compounds.     

Cultivation impacts soil microbial dynamics in dry tropical forest ecosystem in India

We studied for two years the seasonal changes in plant available nitrate and ammonium nitrogen (N), nitrification, N-mineralization, microbial biomass carbon (MBC), nitrogen (MBN) and phosphorus (MBP) in two forest and three cropland sites, derived from a tropical forest ecosystem of India. Results indicated that seasonal values of nitrate N, ammonium N and phosphate P ranged from 7.33–12.99, 5.1–10.22 and 4.0–7.8 μg g^?1 in forest and 4.13–9.26, 9.35–14.46 and 2.8–5.8 μg g^?1 in cropland ecosystems, respectively, with maximum values in summer and minimum in rainy seasons. Nitrification and N-mineralization values varied from 6–28 and 4–26 μg g^?1 mo^?1 in forest and 3–14 μg g^?1 mo^?1 and 4–17 μg g^?1 mo^?1 in cropland, with maximum values in rainy season and minimum in summer season.MBC, MBN MBP ranged from 393–753, 34–80 and 16–36 μg g^?1 in forests and 186–414, 21–41 and 11–22 μg g^?1 in croplands, being maximum in summer and minimum in rainy seasons. There was gradual increase in the values of inorganic N, nitrification, N-mineralization and MBC, MBN and MBP along the age of cropland. Analysis of variance indicated significant difference in the concentration of inorganic N, nitrification and N-mineralization and MBC, MBN and MBP due to sites and seasons.Cultivation caused decline in the mean annual organic C, N and P by 42%, 29% and 13%. The values of nitrate N were decreased by 23–38%, while ammonium N was increased by 39–74%. Nitrification and N-mineralization values were reduced by 39–63% and 40–60%, respectively. Microbial C, N and P were reduced by 44–54%, 41–50% and 28–44%, respectively. Nonetheless, the contribution of soil microbial biomass reflected in total N was enhanced from 4.76% in forest to 5.03% in cropland ecosystem. Enhancement of plant available ammonium-N and microbial contribution in total N are an indicator of natural conserving mechanism to check the nitrogen loss from the nutrient poor agro-ecosystem.     

Budesonide quantification by HPLC coupled to atmospheric pressure photoionization (APPI) tandem mass spectrometry. Application to a comparative systemic bioavailability of two budesonide formulations in healthy volunteers

In the present study, a novel, fast, sensitive and robust method to quantify budesonide in human plasma using 3-keto-desogestrel as the internal standard (IS) is described. The analyte and the IS were extracted from human plasma by liquid–liquid extraction (LLE) using ether. Extracted samples were analyzed by high performance liquid chromatography coupled to Atmospheric pressure photoionization tandem mass spectrometry (HPLC–APPI-MS/MS). Chromatography was performed isocratically on a C18, 5 μm analytical column. The temperature of the autosampler was kept at 6 °C and the run time was 4.00 min. A linear calibration curve over the range 7.5–1000 pg ml^?1 was obtained and the lowest concentration quantified was 7.5 pg ml^?1, demonstrating acceptable accuracy and precision. This analytical method was applied in a relative bioavailability study in order to compare a test budesonide 64 μg/dose nasal spray formulation vs. a reference 64 μg/dose nasal spray formulation (Budecort Aqua) in 48 volunteers of both sexes. The study was conducted in an open randomized two-period crossover design and with a one-week washout period. Plasma samples were obtained over a 14 h interval. Since the 90% CI for both C_max, AUC_last and AUC_0-inf were within the 80–125% interval proposed by the Food and Drug Administration and ANVISA, it was concluded that budesonide 64 μg/dose nasal spray was bioequivalent to Budecort Acqua^® 64 μg/dose nasal spray, according to both the rate and extent of absorption.     

Hollow fiber liquid phase microextraction followed by high performance liquid chromatography for determination of ultra-trace levels of Se(IV) after derivatization in urine,plasma and natural water samples

In the present work, a simple and high sensitive method based on hollow fiber liquid phase microextraction (HF-LPME) was developed followed by high performance liquid chromatography (HPLC) for determination of ultra-trace amounts of Se(IV) after derivatization in biological and natural water samples. Se(IV) was complexed with o-phenylenediamine to form piazselenol. The formed piazselenol was extracted into 20 μL of 1-octanol located in the lumen of a hollow fiber and the solution was injected into HPLC-UV for analysis. Using the Taguchi method, an orthogonal array design (OAD), OA₁₆ (4⁵) was employed to optimize the HF-LPME of piazselenol. The effect of five experimental factors (each factor at four levels) including the volume of the organic phase, extraction time, pH of the solution, stirring rate and ionic strength on the extraction efficiency of piazselenol was studied and optimized. The maximum extraction efficiency of piazselenol was obtained at 20 μL of 1-octanol as the extracting solvent, 30 min extraction time, pH 2, stirring rate of 500 rpm and 30% (w/v) NaCl. Under the optimum conditions, preconcentration factors up to 130 were achieved and the relative standard deviation (%RSD) of the method was <3.7% for different concentrations of Se(IV). The calibration curves were obtained in the ranges of 0.2–100 and 0.05–10 μg L^?1 for the 11 and 50 mL of the sample volumes with reasonable linearity, respectively (r² > 0.995). The limits of detection (LOD) were 0.1 and 0.02 μg L^?1 for the 11 and 50 mL sample volumes, respectively (S/N = 3). Finally, the applicability of the proposed method was evaluated by the extraction and determination of Se(IV) in the plasma, urine and water samples.     

Simultaneous determination of quinolones for veterinary use by high-performance liquid chromatography with electrochemical detection

A selective method based on high-performance liquid chromatography with electrochemical detection (HPLC-ECD) has been developed to enable simultaneous determination of three fluoroquinolones (FQs), namely danofloxacin (DANO), difloxacin (DIFLO) and sarafloxacin (SARA). The fluoroquinolones are separated on a Novapack C-18 column and detected in a high sensitivity amperometric cell at a potential of +0.8 V. Solid-phase extraction was used for the extraction of the analytes in real samples. The range of concentration examined varied from 10 to 150 ng g^?1 for danofloxacin, from 25 to 100 ng g^?1 for sarafloxacin and from 50 to 315 ng g^?1 for difloxacin, respectively. The method presents detection limits under 10 ng g^?1 and recoveries around 90% for the three analytes have been obtained in the experiments with fortified samples. This HPLC-ECD approach can be useful in the routine analysis of antibacterial residues being less expensive and less complicated than other more powerful tools as hyphenated techniques.     

On-line preconcentration/determination of zinc from water,biological and food samples using synthesized chelating resin and flame atomic absorption spectrometry

An on-line flow injection pre-concentration-flame atomic absorption spectrometry method was developed to determine trace zinc in water (tap, dam, and well water), biological (hair and nail), and liver samples. As a solid phase extractant, a synthesized new chelating resin, poly(2-thiozylmethacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propane sulfonic acid) was used. The resin was characterized by Fourier transform infrared spectroscopy, elemental analysis, and surface area by nitrogen sorption. A pre-concentration factor of 40-fold for a sample volume of 12.6 mL was obtained by using the time-based technique. The detection limit for the pre-concentration method was found to be 2.2 μg L^?1. The precision (as RSD,%) for 10 replicate determinations at the 0.04 μg mL^?1 Zn concentration was 1.2%. The calibration graph using the pre-concentration system for zinc was linear with a correlation coefficient of 0.998 in the concentration range from 0.005 to 0.05 μg mL^?1. The applicability and accuracy of the developed method were estimated by the analysis spiked water, biological, liver samples (83–105%), and also certified reference material TMDA-70 (fortified lake water) and SPS-WW1 Batch 111-Wastewater. The results were in agreement with the certified values.     

Management scenario evaluation for a large treatment wetland using a spatio-temporal phosphorus transport and cycling model

This paper describes the development of a two-dimensional, spatially distributed model to simulate coupled hydrologic and phosphorus (P) biogeochemical processes in a 147-ha cell of a 1544-ha stormwater treatment wetland designed to help protect the greater Everglades, FL, USA. The model was used to assess the effects of a suite of feasible management alternatives on the long-term ability of the wetland to sustain total P (TP) removal. The spatial and temporal dynamics of TP retention were simulated under historical (1995–2000) conditions, and under assumptions of removal of short-circuiting channels and ditches, changes in external hydraulic and TP loading, and long-term (>20 years) impacts on soil and water column TP dynamics under current and reduced load conditions. Internal hydrology and transport processes were calibrated against measured tracer concentrations, and subsequently validated against outflow discharge and spatial chloride concentration data. Cycling of P was simulated as first-order uptake and release, with different uptake coefficients for open water/sparse submerged aquatic vegetation (SAV) areas (0.2 day^?1) and dense SAV areas (0.4 day^?1), and a much lower, uniform release coefficient (1.97 × 10^?4 day^?1). The calibration and validation of the P model showed good agreement with field measurements of water column TP concentrations measured at the wetland outlet (calibration RMSE = 10.5 μg L^?1; validation RMSE = 15.6 μg L^?1). Under simulated conditions of preferential channels eliminated, average annual TP treatment effectiveness increased by 25%. When inflow TP loads were assumed to be eliminated after 6 years of loading, the release of accumulated soil P sustained predicted annual average outlet concentrations above 6.7 μg L^?1 for 18 years, decreasing at a rate of 0.16 μg L^?1 yr^?1. Sensitivity analyses indicate that the most critical model input factors include flow resistance parameters, initial soil TP content, and P cycling parameters compared to initial water level, initial TP concentration in water column, ET and transport parameters.     

Determination of biogenic amines in beer with pre-column derivatization by high performance liquid chromatography

Eighteen samples of commercially available Chinese beer were analyzed in order to determine the content of biogenic amines. The method involves pre-column derivatization of the amines with 4-chloro-3,5-dinitrobenzotrifluoride (CNBF) and subsequent analysis by RP-HPLC (reversed phase-high performance liquid chromatography) with diode array detection. The labeled biogenic amines were separated on a Kromasil C18 column (250 mm × 4.6 mm, 5 μm) at room temperature and UV detection was applied at 254 nm. The separation of seven labeled biogenic amines was achieved within 22 min by elution acetonitrile and HAc–NaAc buffers. The method linearity, calculated for each biogenic amine, has a correlation coefficient higher than 0.9925, in concentrations ranging from 2.9 μmol L^?1 to 565 μmol L^?1. Detection limits of biogenic amines were 0.056–0.87 μmol L^?1, at a signal-to-noise ratio of 3. The proposed method has been applied to the quantitative determination of spermine, phenethylamine, spermidine, histamine, tyramine, tryptamine and putrescine in beer with recoveries of 91.9–103.1% and R.S.D. of 2.86–5.63%. Quantitation is relative to external standards. The results showed that each kind of beer examined contained at least three biogenic amines. Putrescine, histamine and tyramine were detected in all samples. Spermidine was detected in 89% of the beers. Spermine, tryptamine and phenylethylamine occurred in 78%, 61% and 44% of the beers examined, respectively. These levels were below the level that may elicit direct adverse reactions for most consumers.     

Production of yeast chitin–glucan complex from biodiesel industry byproduct

Crude glycerol from the biodiesel industry was used as carbon source for high cell density fed-batch cultivation of Pichia pastoris aiming at producing a chitin–glucan complex (CGC). More than 100 g L^?1 biomass was obtained in less than 48 h. The yield of biomass on a glycerol basis was 0.55 g g^?1 during the batch phase and 0.63 g g^?1 during the fed-batch phase. The chitin–glucan complex was recovered from the yeast cell wall by hot alkaline extraction. CGC content in the cell wall was found to be relatively constant throughout the cultivation (18–26%) with a volumetric productivity of 1.28 g L^?1 h^?1 at the end of the fed-batch phase. The molar ratio of chitin:β-glucan in the extracted biopolymer was 16:84, close to other CGC extracted from Aspergillus biomass. The extracted polymer was characterized by Differential Scanning Calorimetry (DCS) and solid-state Nuclear Magnetic Resonance (NMR) spectroscopy and compared with commercial biopolymers, namely, crab shell chitin and/or chitosan, algal β-glucan (laminarin) and fungal chitin–glucan complex (kiOsmetine).     

Determination of phenothiazine derivatives in human urine by using ionic liquid-based dynamic liquid-phase microextraction coupled with liquid chromatography

A simple and rapid method for the determination of seven phenothiazines derivatives (chlorpromazine, promethazine, levomepromazine, prochlorperazine, trifluoperazine, fluphenazine and thioridazine) in human urine samples is presented. The analytes are extracted from the sample in 50 μL of the ionic liquid 1-butyl-3-methyl-imidazolium hexafluorophosphate working in an automatic flow system under dynamic conditions. The chemical affinity between the extractant and the analytes allows a good isolation of the drugs from the sample matrix achieving at the same time their preconcentration. The separation and detection of the extracted compounds is accomplished by liquid chromatography and UV detection. The proposed method is a valuable alternative for the analysis of these drugs in urine within the concentration range 0.07–10 μg mL^?1. Limits of detection were in the range from 21 ng mL^?1 (thioridazine) to 60 ng mL^?1 (levomepromazine). The repeatability of the proposed method expressed as RSD (n = 5) varied between 2.2% (levomepromazine) and 3.9% (chlorpromazine).     

Coupled effects of irradiance and iron on the growth of a harmful algal bloom-causing microalga Scrippsiella trochoidea

Effects of irradiance and iron on the growth of a typical harmful algal blooms (HABs) causative dinoflagellate, Scrippsiella trochoidea, were investigated under various irradiances (high light: 70 μmol m^?2 s^?1 and low light: 4 μmol m^?2 s^?1) and iron concentrations (low iron: 0.063 mg L^?1, medium iron: 0.63 mg L^?1 and high iron: 6.3 mg L^?1), and evaluated by the parameters of algal cell density, specific growth rate, optical density and chlorophyll a content. The results indicated that there was significant difference in the cell density of dinoflagellate S. trochoidea between high light and low light intensity treatments across the entire experiments, 7-fold higher at high irradiance as compared with low irradiance, which was further enhanced by the iron concentration. It was found that the maximum cell density of 25 × 10⁴ cell mL^?1 occurred under the combination of high light intensity and high iron concentration, followed by 23 × 10⁴ cell mL^?1 in the combination of high light and medium iron, and 20 × 10⁴ cell mL^?1 in the combination of high light and low iron. There was no significant effect of iron concentration on the cell density under low light intensity. The cell density maintained about 3 × 10⁴ cell mL^?1 across all combinations of iron concentrations and low light in the end of experiments. Such interactive effects of light intensity and iron level dependent were also observed for the specific growth rate, OD₆₈₀ and chlorophyll a content of S. trochoidea. The maximum values of specific growth rate, OD₆₈₀ and chlorophyll a content peaked at the condition of high irradiance and high iron, which were 0.22 d^?1, 0.282 and 0.673 mg L^?1, respectively. In general, their values increased significantly with the increasing of iron concentration at high irradiance, whereas no significant difference was observed among three iron concentrations at low irradiance, all remaining approximately 0.06 d^?1, 0.03 and 0.050 mg L^?1, respectively. Those results suggest that there may be a strong interactive effect between irradiance and iron on microalgal growth and their physiological characteristics. The combination of high light and high iron concentration may accelerate algal cell growth and pigment biosynthesis, thus leading to massive occurrence of HABs.     

Extraction of trace amounts of pioglitazone as an anti-diabetic drug with hollow fiber liquid phase microextraction and determination by high-performance liquid chromatography-ultraviolet detection in biological fluids

The applicability of hollow fiber liquid phase microextraction (HF-LPME) for extraction and preconcentration of trace amounts of pioglitazone (PGL) as an anti-diabetic drug in biological fluids, prior to determination by high-performance liquid chromatography (HPLC), was evaluated. In this technique, the target drug was extracted into di-n-hexyl ether immobilized in the wall pores of a porous hollow fiber from 10 mL of the aqueous sample (source phase, SP) with pH 8.0, and then back extracted into the receiving phase (RP) with pH 2.2 located in the lumen of the hollow fiber. The extraction occurred due to a pH gradient between the two sides of the hollow fiber. After extracting for a prescribed time, 24 μL of the RP solution was taken back into the syringe and injected directly into a HPLC instrument for quantification. The Taguchi orthogonal array (OAD) experimental design with an OA₁₆ (4⁵) matrix was employed to optimize the HF-LPME conditions. Different factors affecting the HF-LPME efficiency such as the nature of organic solvent used to impregnate the membrane, pH of the SP and RP, stirring speed, extraction time and ionic strength were studied and optimized. Under the optimum conditions (di-n-hexyl ether as membrane impregnation solvent, pHs of the SP and RP equal to 8.0 and 2.2, respectively, extraction time of 30 min, stirring speed of 500 rpm and 10% (w/v) NaCl for adjusting the ionic strength), preconcentration factor of 180, linear dynamic range (LDR) of 2.5–250 μg L^?1 with good correlation of determination (r² > 0.998) and limit of detection (LOD) of 1.0 μg L^?1 were obtained for the target drug. The percent relative intra-day and inter-day standard deviations (RSDs%) based on five replicate determinations were 4.7 and 15%, respectively. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of PGL in different types of biological fluids such as plasma and urine samples. The results showed that the proposed HF-LPME method could be successfully applied to determine trace amounts of PGL in biological samples.     

Serum selenium levels of the very low birth weight premature newborn infants with bronchopulmonary dysplasia

BackgroundThe selenium (Se) is an essential trace element that has a critical role in synthesis and activity of a number of selenoproteins with protective properties against free radical damage. This study was conducted to detect the serum Se concentration in very low birth weight (VLBW) preterm infants and its association with bronchopulmonary dysplasia (BPD).Materials and methodsCord blood Se concentration was determined in 54 neonates with gestation age 30 week or less. Another sample was obtained from these infants at day 28 of birth and serum Se levels were measured by atomic absorption spectrophotometer. All neonates were followed for oxygen dependency at 28 day after birth and 36 week postmenstrual age.ResultsThe mean cord blood Se concentration in studied neonates was 64.78 ± 20.73 μg L^?1. Serum Se concentration was 60.33 ± 26.62 μg L^?1 at age 28-day. No significant correlation was observed for serum Se concentration at birth and at one month after birth (r = ?0.04, p = 0.72). BPD was diagnosed in 25 neonates (46%). The mean serum Se concentration at one month was 57.16 ± 29.68 μg L^?1 in patients with BPD (25 cases) and 63.27 ± 23.6 μg L^?1 in 29 patients without BPD (p = 0.40).ConclusionIn our study, serum Se concentration at 28 day of birth was lower than cord blood levels in preterm neonates, but we have not found significant difference among patients who had BPD or not with respect to serum Se concentrations at this age.     

Treatment of acidic wastewater arising from the refining of vegetable oil by crossflow microfiltration at very low transmembrane pressure

The refining process of vegetable oils generates acidic wastewater with the following characteristics: pH (1–1.5), COD (10–30 g O₂ L⁻¹), suspended solids (7–12 g L⁻¹) and fats (2–4 g L⁻¹). In order to reduce the effluent load and recover a fraction of the fats without using any additives, a microfiltration (0.2–1.4 μm) process involving ceramic membranes at very low transmembrane pressure values (0.1–1 bar) was assessed. Four batches of acidic wastewater from different manufacturing runs were tested. Trials with a constant volumetric reduction ratio of 30 were carried out for periods of more than 5 h. With a 0.5 μm membrane it was possible to maintain a permeate flux of 100 L h⁻¹ m⁻² for 24 h and achieve a 91% reduction in SS, a 96% reduction in fat and a COD reduction of more than 60%. In addition, the retentate thus extracted separated spontaneously into two phases, both of which could be exploited: the upper phase mainly consisting of fats as a by-product and the lower clarified phase which could be mixed into the permeate.