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1.
Sci Rep ; 14(1): 8027, 2024 04 05.
Article in English | MEDLINE | ID: mdl-38580764

ABSTRACT

The aim of this study was to assess the effects of substituting traditional forage fiber sources with cottonseed cake in the diet on both the quantitative and qualitative characteristics of carcass and meat in Nelore young bulls. Twenty-four Nelore steers starting with an average weight of 377.8 ± 43.5 kg, were individually housed in stalls and provided with individualized feeding over a 112-day confinement period. The study followed a completely randomized design with two treatments and 12 replications. The diets incorporated either whole plant corn silage (WPCS) and, cottonseed cake (CSC) as fiber sources, at a rate of 300 g/kg of dry matter. The CSC diet promoted higher carcass weight. Aging animal meat for seven days significantly decreased the shear force from 83.4 to 71.6 N. Although diets did not influence meat composition, WPCS diet provided higher concentrations of C16:1, C18:1n9c, C18:3n3, and C22:2 acid, and CSC diet higher concentrations of C15:0, C18:1n9t, C18:2n6c, and 20:3n3. The WPCS diet provided higher concentrations of monounsaturated fatty acids and ω9, and the CSC diet had higher concentrations of ω6 and ω6:ω3 ratio in meat. Cottonseed cake used as a fiber source increases the concentration of polyunsaturated fatty acids and ω6 fatty acids in the meat of young bulls finished in feedlot.


Subject(s)
Animal Feed , Cottonseed Oil , Male , Animals , Cattle , Animal Feed/analysis , Animal Nutritional Physiological Phenomena , Diet/veterinary , Meat/analysis , Zea mays
2.
Biomed Pharmacother ; 174: 116308, 2024 May.
Article in English | MEDLINE | ID: mdl-38626517

ABSTRACT

The kernel oil of the Attalea phalerata Mart. Ex Spreng (Acurí) is traditionally used in several Latin American countries to treat respiratory problems, inflammation, and fever. However, it cannot be found on the literature any attend to use this oil in pharmaceutical formulation. In this paper, it was developed Acurí oil-loaded nanocapsules, and it was evaluated the cytotoxicity against cancer cells, the antinflammatory activity and the oral acute toxicity in rats. Acurí oil contains lauric acid as the predominant saturated fatty acid (433.26 mg/g) and oleic acid as the main unsaturated fatty acid (180.06 mg/g). The Acurí oil-loaded nanocapsules showed a size of 237 nm, a polydispersity index of 0.260, and a high ζ-potential of -78.75 mV. It was obtained an encapsulation efficiency of 88.77%, and the nanocapsules remain stable on the shelf for 180 days. The nanocapsules showed a rapid release profile (98.25% in 40 minutes). Nanocapsules at a dose of 10 mg/kg exhibit an anti-inflammatory effect similar to indomethacin at the same dose. The nanocapsules showed excellent antiproliferative effect and selectivity index against prostate tumor cells (IC50 2.09 µg/mL, SI=119.61) and kidney tumor cells (IC50 3.03 µg/mL, SI=82.50). Both Acurí oil and Acurí oil-loaded nanocapsules are nontoxic at a dose of 2000 mg/kg. Additionally, they reduce serum triglyceride and total cholesterol levels in rat and could find application in nutraceutical formulations. The Acurí oil-loaded nanocapsules emerge as a promising candidate for new antitumor therapies.


Subject(s)
Anti-Inflammatory Agents , Nanocapsules , Plant Oils , Animals , Anti-Inflammatory Agents/pharmacology , Anti-Inflammatory Agents/isolation & purification , Anti-Inflammatory Agents/administration & dosage , Plant Oils/pharmacology , Male , Humans , Rats , Rats, Wistar , Administration, Oral , Cell Line, Tumor
3.
Trop Anim Health Prod ; 55(2): 109, 2023 Mar 14.
Article in English | MEDLINE | ID: mdl-36917307

ABSTRACT

The objective was to evaluate the effect of the supplementation with natural antioxidants from Yerba mate (Ilex paraguariensis St. Hil.) on the performance, carcass and meat characteristics, and fatty acid profile in meat and fat of Texel × Ile de France lambs kept in Brachiaria-grass pasture. Twenty lambs with a mean age of 90 days and 26.3 kg of BW were distributed in a completely randomized design in two treatments with 10 replicates/treatment: Control-protein-energy supplement based on corn and soybean meal (150 g/kg DM of crude protein) without the addition of natural antioxidant yerba mate and Yerba Mate - energy protein supplement with the addition of yerba mate (110 g/kg DM). There was no treatment effect on animal performance and carcass characteristics. The subcutaneous fat thickness was significantly higher for lambs treated without yerba mate. There was no effect of nutritional treatments on the oxidative markers of lamb meat. The muscle of the animals treated with yerba mate showed a higher concentration of unsaturated and polyunsaturated fatty acids elaidic, linolenic, thymnodonic, docosadienoic, and ceorvonic. The fat of the animals treated with yerba mate showed a higher concentration of palmitoleic acid, linoelaidic acid, heneicosanoic acid, dihomo-γ-linolenic acid, and arachidonic acid. The concentration of polyunsaturated fatty acids was significantly higher in meat and fat of lambs treated with yerba mate. Including yerba mate in the diet of lambs kept on Brachiaria pastures improves the lipid profile of polyunsaturated fatty acids in meat and fat, without altering the performance of the animals.


Subject(s)
Ilex paraguariensis , Animals , Animal Feed/analysis , Antioxidants , Fatty Acids/metabolism , Fatty Acids, Unsaturated , Ilex paraguariensis/metabolism , Meat/analysis , Sheep , Sheep, Domestic/metabolism
4.
Trop Anim Health Prod ; 55(1): 13, 2022 Dec 19.
Article in English | MEDLINE | ID: mdl-36534328

ABSTRACT

The hypothesis tested is that the association of soybean grain and yerba mate as an antioxidant source can increase the concentration of polyunsaturated fatty acids (PUFA) with lower oxidation of milk from lactating ewes reared in tropical pastures. Sixteen ewes were randomly distributed in a 2x2 factorial scheme (with or without yerba mate at 110 g / kg of dry matter (DM); with or without soybean grain at 210 g/kg of DM). Yerba mate intake reduced DM intake, and concentrations of ether extract (EE), protein, lactose, defatted dry extract, density, omega-3 concentrations, and the ratio between saturated/monounsaturated fatty acids (FA), but increased the concentration of monounsaturated FA and the sequestering power of free radicals by DPPH without altering the concentrations of conjugated dienes and the concentrations of substances reactive to thiobarbituric acid in milk. Supplementation with soybean grain decreased the birth weight of the lambs and increased the concentrations of conjugated linoleic acid (CLA), PUFA, omega - 6, omega ratio - 6/omega - 3, and total blood cholesterol. The addition of yerba mate did not influence the oxidative profile of milk. Supplementation with soybean grain improved the FA profile of milk, increasing the concentrations of CLA and PUFA. The results suggest that the association of yerba mate and soybean grain helps to improve the fat quality of milk from ewes raised in tropical pastures, as shown by the enhanced antioxidant activity, although it does not help prevent oxidation of milk rich in PUFA.


Subject(s)
Antioxidants , Ilex paraguariensis , Animals , Female , Antioxidants/metabolism , Dietary Supplements , Edible Grain , Fatty Acids/analysis , Fatty Acids, Unsaturated/analysis , Ilex paraguariensis/chemistry , Lactation , Milk/chemistry , Plant Extracts/chemistry , Sheep , Glycine max
5.
Molecules ; 27(19)2022 Oct 08.
Article in English | MEDLINE | ID: mdl-36235241

ABSTRACT

BACKGROUND: Studies indicate that different parts of Carica papaya Linn have nutritional properties that mean it can be used as an adjuvant for the treatment of various pathologies. METHODS: The fatty acid composition of the oil extracted from the seeds of Carica papaya Linn was evaluated by gas chromatography, and an acute toxicity test was performed. For the experiment, Swiss mice were fed a balanced or high-fat diet and supplemented with saline, soybean oil, olive oil, or papaya seed oil. Oral glucose tolerance and insulin sensitivity tests were performed. After euthanasia, adiposity, glycemia, total cholesterol and fractions, insulin, resistin, leptin, MCP-1, TNF-α, and IL-6 and the histology of the liver, pancreas, and adipose tissue were evaluated. RESULTS: Papaya seed oil showed predominance of monounsaturated fatty acids in its composition. No changes were observed in the acute toxicity test. Had lower food intake in grams, and caloric intake and in the area of adipocytes without minimizing weight gain or adiposity and impacting the liver or pancreas. Reductions in total and non-HDL-c, LDL-c, and VLDL-c were also observed. The treatment had a hypoglycemic and protective effect on insulin resistance. Supplementation also resulted in higher leptin and lower insulin and cytokine resistance. CONCLUSIONS: Under these experimental conditions, papaya seed oil led to higher amounts of monounsaturated fatty acids and had hypocholesterolemic, hypotriglyceridemic, and hypoglycemic effects.


Subject(s)
Carica , Adiposity , Animals , Carica/chemistry , Cholesterol, LDL , Diet, High-Fat/adverse effects , Fatty Acids/analysis , Fatty Acids, Monounsaturated , Hypoglycemic Agents/analysis , Insulin , Interleukin-6/analysis , Leptin , Mice , Obesity , Olive Oil/analysis , Resistin , Seeds/chemistry , Soybean Oil/analysis , Tumor Necrosis Factor-alpha
6.
Nutrients ; 14(12)2022 Jun 19.
Article in English | MEDLINE | ID: mdl-35745276

ABSTRACT

Mauritia flexuosa (Buriti) pulp oil contains bioactive substances and lipids that are protective against cardiovascular and inflammatory diseases. We performed physical and chemical analyses to verify its quality and stability. Buriti oil was stable according to the Rancimat test, presenting an induction period of 6.6 h. We evaluated the effect of supplementation with crude buriti oil and olive oil on metabolic parameters in 108 Swiss mice for 90 days. We investigated six groups: extra virgin olive oil (EVOO) 1 and 2 (1000 and 2000 mg/kg), buriti oil (BO) 1 and 2 (1000 and 2000 mg/kg), synergic (S) (BO1 + EVOO1), and control (water dose 1000 mg/kg). The animals were euthanized to examine their blood, livers, and fats. The supplementation did not interfere with food consumption, weight gain, and histological alterations in the liver. Group S showed the strongest relationship with the fractions HDL-c and non-HDL-c, indicating a possible cardioprotective effect. Moreover, we observed significantly higher IL-6 levels in the control, EVOO2, and BO1 groups than in the EVOO1 group. Resistin was also significantly higher for the synergic treatment than for the control. We conclude that BO combined with EVOO could be an excellent food supplement for human consumption.


Subject(s)
Arecaceae , Animals , Arecaceae/chemistry , Dietary Supplements , Liver/metabolism , Mice , Models, Theoretical , Olive Oil/metabolism , Plant Oils/chemistry
7.
PLoS One ; 17(2): e0263071, 2022.
Article in English | MEDLINE | ID: mdl-35171914

ABSTRACT

Studies comparing methodologies for fatty acids are very important, since they can influence the quality and final quantification of the lipid fraction. Objective-to compare different extraction methods for total lipids and to evaluate the effect of these methodologies on the quantitative composition of fatty acids in milk of lactating ewes raised in tropical pastures. The methodologies used were simple direct transesterification, using the HPLC grade organic solvent n-hexane, Bligh; Dyer (cold extraction, extracting mixture proportions 5, 10, and 15 mL in a ratio of 2:1:1 (v/v/v) of chloroform-methanol-water). The fatty acid methyl esters were separated by gas chromatography coupled with a flame ionization detector (GC-FID). The results show that there was no significant difference (p <0.05) in the total lipid content between the extraction methods. However, the Bligh's method; Dyer obtained the best yield of lipids to be extracted from ewe's milk, since the volume with 15 mL of the extraction solution was able to identify 87% of the chromatographic peaks. It was also observed that ewe's milk has a higher percentage of palmitic, stearic and oleic fatty acids, with percentages of 20.1%, 15.5% and 33.1%, respectively. Therefore, an extraction mixture with a volume of 15 mL used in this study may be an alternative to perform the extraction of milk fat from high lactating ewes in tropical pastures as a routine method, as it expresses the best lipid content of this food.


Subject(s)
Fatty Acids/analysis , Fatty Acids/isolation & purification , Milk/chemistry , Solvents/chemistry , Water/chemistry , Animals , Chromatography, High Pressure Liquid , Esterification , Female , Lactation , Sheep
8.
J Med Food ; 24(8): 841-851, 2021 Aug.
Article in English | MEDLINE | ID: mdl-34342510

ABSTRACT

Obesity is a relevant health hazard characterized as a chronic noncommunicable disease, with severe comorbidities that cause mortality worldwide. Acrocomia aculeata is a Brazilian palm with edible fruits. Its pulp contains fibers, monounsaturated fatty acids (MUFAs), such as oleic acid and carotenoids. In this context, our study aimed to elucidate the protective effect of the lyophilized A. aculeata pulp added at the rates of 1%, 2%, and 4% to a high-fat (HF) diet (rich in saturated fats and cholesterol), for 90 days, in mice. The treatment with 4% pulp induced a significant increase in the biochemical parameters of serum cholesterol HDL-C (high-density lipoprotein) compared with the control. According to the evaluation of the epididymal tissue, the groups treated with A. aculeata pulp exhibited smaller fat deposits compared with the HF diet group. Therefore, we infer that the predominant components in A. aculeata, particularly fibers and MUFAs, promote beneficial effects on health parameters during simultaneous exposure to food rich in saturated fat and cholesterol, typical of the Western diet. This is the first study to correlate the presence of fatty acids from A. aculeata pulp in different proportions added in a HF diet with metabolic and histological parameters in Swiss mice.


Subject(s)
Diet, High-Fat , Dietary Fats , Adipocytes , Animals , Cholesterol , Diet, High-Fat/adverse effects , Fatty Acids, Monounsaturated , Hypertrophy , Lipoproteins, HDL , Mice
9.
Food Res Int ; 144: 110362, 2021 06.
Article in English | MEDLINE | ID: mdl-34053555

ABSTRACT

Problems related to oil authenticity make it difficult to obtain the benefits associated with each type of vegetable oil. Fraudulent practices have been revealed by several targeted and nontargeted methods. In this paper, spectroscopic techniques (FT-IR, 1H NMR, and 13C NMR) were applied to determine the chemical profiles of 23 Brazilian commercial vegetable oils obtained from five different high-value aggregated matrices (andiroba, babassu, baru, castor, and sweet almond oils) and investigate their adulteration, by comparison with the corresponding reference samples. Each technique is useful for the particular information it provides: differences in free fatty acids by FT-IR; adulteration with omega-3-enriched oils by 1H NMR, and adulteration of unsaturated-enriched oil with another unsaturated oil without linoleic acid by regiospecific analysis. Our findings highlight the importance of fusion-based methods in providing precise information for use in oil quality authentication.


Subject(s)
Food Contamination , Plant Oils , Brazil , Food Contamination/analysis , Plant Oils/analysis , Proton Magnetic Resonance Spectroscopy , Spectroscopy, Fourier Transform Infrared
10.
J Anim Physiol Anim Nutr (Berl) ; 105(2): 364-375, 2021 Mar.
Article in English | MEDLINE | ID: mdl-33226712

ABSTRACT

Metabolic syndrome (MetS) and obesity are growing in many parts of the world, becoming public health problems. It is proposed that foods with functional properties can assist in the treatment of these diseases. Crude buriti pulp oil (BPO) is a food traditionally consumed by residents in the Pantanal, Cerrado and Brazilian Amazon. It is rich in oleic acid, tocopherols and carotenoids, emerging as a potential functional food. Thus, this study aimed to evaluate the effect of the supplementation of BPO on metabolic disorders caused by a high-fat diet. Four groups of C57BL6 mice were used, a lean group with AIN-93M diet and control oil supplementation, an obese group with a high-fat diet and control oil supplementation, and two obese groups with a high-fat diet and BPO supplementation in the amounts of 50 and 100 mg/kg. BPO worsened the metabolic state caused by the high-fat diet, worsening risk factors associated with MetS, as the abdominal circumference and retroperitoneal fat, serum levels of total cholesterol, uric acid, alanine transaminase, glucose and triglycerides, and renal fat, in addition to changes in glycaemic control and oxidative stress markers. C57BL/6 mice fed with a high-fat diet and supplemented with BPO presented a worsening in metabolic risk factors associated with MetS.


Subject(s)
Metabolic Diseases , Rodent Diseases , Animals , Carotenoids , Diet, High-Fat/adverse effects , Liver , Metabolic Diseases/veterinary , Mice , Mice, Inbred C57BL
11.
Molecules ; 25(19)2020 Oct 03.
Article in English | MEDLINE | ID: mdl-33022905

ABSTRACT

The fruit of Caryocar brasiliense Cambess. is a source of oil with active compounds that are protective to the organism. In our work, we analyzed the physicochemical characteristics and evaluated the effects of supplementation with C. brasiliense oil in an animal model. We characterized the oil by indices of quality and identity, optical techniques of absorption spectroscopy in the UV-Vis region and fluorescence, and thermogravimetry/derived thermogravimetry (TG/DTG). For the animal experiment, we utilized mice (Mus musculus) supplemented with lipidic source in different dosages. The results demonstrated that C. brasiliense oil is an alternative source for human consumption and presents excellent oxidative stability. Primarily, it exhibited oleic MFA (53.56%) and palmitic SFA (37.78%). The oil level of tocopherols and tocotrienols was superior to the carotenoids. The supplementation with C. brasiliense oil reduced the levels of total cholesterol, LDL-c, and non-HDL-c. Regarding visceral fats and adiposity index, the treatment synergically supplemented with olive oil and C. brasiliense oil (OO + CO) obtained the best result. Therefore, C. brasiliense oil is a high quality product for consumption. Its supplementation promotes beneficial effects mainly on the lipidic profile.


Subject(s)
Cholesterol, LDL/metabolism , Dietary Supplements , Ericales/chemistry , Lipoproteins, HDL/metabolism , Plant Oils/pharmacology , Animals , Body Weight/drug effects , Electric Conductivity , Fatty Acids/analysis , Male , Organ Size/drug effects , Thermogravimetry
12.
Magn Reson Chem ; 58(2): 186-190, 2020 02.
Article in English | MEDLINE | ID: mdl-31663181

ABSTRACT

High sodium dietary intake has a positive association with an increase in blood pressure and can be correlated with risk factors of disease. Considering that the World Health Organization recommends a sodium intake lower than 2 g day-1 for adults, the hidden sodium content in processed foods is an important factor that compromises the assessment of a healthy diet. Accordingly, the present paper aimed to quantitate the sodium content of conventional soft drinks and their diet versions using nuclear magnetic resonance spectroscopy as a quantitative analytical technique (23 Na qNMR). The results show one free sodium signal (Na+ ) displayed as a singlet at 0 ppm in the 23 Na NMR spectrum, making its quantitation highly specific. This signal alone was used to directly determine the concentration of sodium in soft drinks. Flame photometry analysis was used to validate the method, and an excellent linearity was found in qNMR analysis (r = 0.9994) in comparison with flame photometry (r = 0.9958). In addition, a good correlation was found between sodium concentrations obtained by 23 Na NMR and flame photometry in the evaluated commercial soft drinks. Since the intensity of the resonance line is directly proportional to the number of nuclei (spins), the concentration of sodium in soft drinks can be determined via this straightforward method without the need for external calibration. The experimental acquisitions are fast (approximately 15 min), allowing the analysis of several samples in a short period of time. This is a novel alternative for sodium quantitation using an efficient NMR methodology.


Subject(s)
Carbonated Beverages/analysis , Magnetic Resonance Spectroscopy/methods , Sodium, Dietary/analysis , Limit of Detection , Reproducibility of Results
13.
Data Brief ; 26: 104427, 2019 Oct.
Article in English | MEDLINE | ID: mdl-31516950

ABSTRACT

Dersani® and sunflower® oils are used by the Brazilian population as a cicatrizing agent. However, data on physical and chemical properties of these oils are scarce. In this data article on oils, we determined a total of 14 fatty acids composition by gas chromatography (GC), as well as quantifying the elements contents (Ca, K, Mg, Al, Cr, Fe, Mn, Na, P, Se and Zn) using inductively coupled plasma optical spectrometry (ICP OES). Rancimat method was used to determine the oxidative stability of the oils at temperature of 110 °C, in which the induction times for Dersani® and Sunflower® oils were 1.54 (±0.02) and 6.21 (±0.17) hours, respectively. Spectroscopic techniques UV-VIS and fluorescence were employed to obtain spectral datasets. UV-VIS and fluorescence spectroscopy reveals the presence of phenolic, tocopherols, tocotrienols and methyl-linolenate compounds in the oils. The determination of mineral and others contents in oils is an important criterion for the assessment of oil quality with regard to oxidation and their toxicity, properties and storage.

14.
Pestic Biochem Physiol ; 148: 22-27, 2018 Jun.
Article in English | MEDLINE | ID: mdl-29891373

ABSTRACT

Temephos is considered the gold standard by the Ministry of Health for controlling the larvae of the mosquito Aedes aegypti. The present study evaluated the effects of Temephos larvicide on the reproductive performance, embryo-fetal development and DNA integrity of Swiss mice. This study used 30 pregnant female mice: 10 were controls treated with drinking water at a dosage of 0.1 mL/10 g (body weight - b.w., administered orally - a.o.), and 20 were treated with Temephos at doses of 0.0043 mg/kg and 0.043 mg/kg (b.w., a.o.) during the gestational period. Statistical analysis showed that Temephos did not alter the biometric or reproductive parameters. Comparing the weight of the fetus to the stage of pregnancy demonstrated that the 0.0043 mg/kg dosage increased the size of the fetuses. No external malformations were detected. However, the 0.043 mg/kg dosage induced changes in the sternum, with the main change being the center of the sternum, xiphoid processes and absence of the manubrium. The other skeletal and visceral alterations did not differ from the control group and are considered variants of normality. The analysis of head measurements showed an increase in the anterior/posterior measurements of the glabella, the external occipital protuberance and the biauricular plane. The circumference and area of the head did not present significant differences. The micronucleus test showed only a 0.043 mg/kg increase in 48 h. Thus, it is considered that Temephos has a low teratogenic and genotoxic risk.


Subject(s)
Aedes/drug effects , DNA/drug effects , Embryonic Development/drug effects , Fetus/drug effects , Insecticides/toxicity , Larva/drug effects , Reproduction/drug effects , Temefos/toxicity , Abnormalities, Drug-Induced , Aedes/growth & development , Animals , Body Weight/drug effects , DNA Damage , Dose-Response Relationship, Drug , Female , Insecticides/metabolism , Mice , Micronucleus Tests , Mutagens/toxicity , Organ Size/drug effects , Placenta/metabolism , Pregnancy , Temefos/metabolism , Teratogens/toxicity , Uterus/drug effects
15.
Article in English | MEDLINE | ID: mdl-27866844

ABSTRACT

The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche.


Subject(s)
Chemical Fractionation , Graphite , Ionic Liquids , Magnets , Molecular Imprinting , Phase Transition
16.
J Sep Sci ; 37(15): 1903-10, 2014 Aug.
Article in English | MEDLINE | ID: mdl-24838528

ABSTRACT

Analyses in chromatographic systems able to save mobile and stationary phases without reducing efficiency and resolution are of current interest. These advantages regarding savings have challenged us to develop a system dedicated to miniaturized liquid chromatography. This paper reports on the development of a high-pressure syringe-type pump, an oven able to perform isothermal and temperature programming and a software program to control these chromatographic devices. The experimental results show that the miniaturized system can generate reproducible and accurate temperature and flow rate. The system was applied to the separation of statins and tetracylines and showed excellent performance.


Subject(s)
Amino Acids/isolation & purification , Chromatography, Liquid/instrumentation , Tetracycline/isolation & purification , Chromatography, Liquid/methods , Temperature
17.
J Sep Sci ; 34(4): 436-45, 2011 Feb.
Article in English | MEDLINE | ID: mdl-21298783

ABSTRACT

This paper presents the development of a procedure, which enables the analysis of nine pharmaceutical drugs in wastewater using gas chromatography-mass spectrometry (GC-MS) associated with solid-phase microextraction (SPME) for the sample preparation. Experimental design was applied to optimize the in situ derivatization and the SPME extraction conditions. Ethyl chloroformate (ECF) was employed as derivatizing agent and polydimethylsiloxane-divinylbenzene (PDMS-DVB) as the SPME fiber coating. A fractional factorial design was used to evaluate the main factors for the in situ derivatization and SPME extraction. Thereafter, a Doehlert matrix design was applied to find out the best experimental conditions. The method presented a linear range from 0.5 to 10 µg/L, and the intraday and interday precision were lower than 16%. Applicability of the method was verified from real influent and effluent samples of a wastewater treatment plant, as well as from samples of an industry wastewater and a river.


Subject(s)
Drug Residues/analysis , Drug Residues/isolation & purification , Sewage/analysis , Solid Phase Microextraction/methods , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/isolation & purification , Gas Chromatography-Mass Spectrometry
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