Chemometric investigation of the effects of chemical properties and concentrations on the extractability of benzimidazoles with supported liquid membrane

Principle component analysis (PCA) and a two-way analysis of variance (ANOVA) were employed in the study of factors affecting extractability of benzimidazole anthelmintics using supported liquid membrane (SLM) in liver, kidney, milk and urine at four concentration levels. The SLM extraction process was monitored by liquid chromatography - mass spectrometer (LC-MS). The results showed that the extractability of benzimidazoles is dependent on both the concentration levels and the chemical properties of compounds. Based on chemical properties, extraction of the compounds from the liver matrix showed no significant difference (p = 0.05) for the following pairs; albendazole and oxibendazole, thiabendazole and mebendazole, oxibendazole and fenbendazole, and oxibendazole and mebendazole. At some of the concentration levels, mainly between 1000 and 100, 100 and 10, and 10 and 1 μg/Kg, there was no significant difference. It was also found that, there was significant difference (at p = 0.05) in the extractability in milk between oxibendazole and albendazole, and also oxibendazole and fenbendazole. For milk also, the concentration range from 10 to 100 μg/L, showed no significant difference (p = 0.05). Urine matrix on the other hand, showed significant difference in the recoveries at all concentration levels

Solid-phase extraction and high performance liquid chromatography with diode array detection method for the determination of antibiotic residues in poultry tissues

This article presents information on high performance liquid chromatography with diode array detection (HPLC-DAD) method for the simultaneous determination of six antibi- otic residues (enrofloxacin, sulfadimethoxine, sulfamerazine, sulfamethoxazole, sulfamox- ole, and tylosin) in three poultry tissues. The target antibiotic residues were extracted from raw poultry samples following concentration, clean-up through solid phase extraction. The data describe the extraction, determination and screening procedures of these common antibiotic residues in 111 samples of fresh and frozen poultry meats. The limit of detection (LOD) ranged from 5.37–55.4 ng/g, while the quantification limit (LOQ) was in the range of 17.9–184 ng/g, respectively, with minimal matrix effect. The calibration curves obtained exhibited a good linear response with the coefficient of determination, R 2 > 0.996. Some concentrations exceeded their maximum residue limits in most samples. These findings indicated elevated levels of antibiotic residues in tissues of locally produced and illegally imported poultry meat samples

Cytotoxicity, phytochemical analysis and antioxidant activity of crude extracts from Rhizomes of Elephantorrhiza Elephantina and Pentanisia Prunelloides

Background: Elephantorrhiza elephantina (Ee) and Pentanisia prunelloides (Pp) are two medicinal plants which are widely used to remedy various ailments including diarrhoea, dysentery, inflammation, fever, rheumatism, heartburn, tuberculosis, haemorrhoids, skin diseases, perforated peptic ulcers and sore joints in southern Africa (South Africa, Swaziland, Botswana and Zimbabwe). The following study was conducted to explore the in vitro cytotoxicity, antioxidant properties and phytochemical profile of the two medicinal plants. Materials and Methods: The cytotoxicity of the aqueous and methanol extracts and fractions of both species was studied using the brine shrimp lethality tests (BST) for the first time. Results: The results demonstrated that the lethality (LC50) for crude extracts for both plants ranged between 1.8 and 5.8 ppm and was relatively greater than that for the methanol, ethyl acetate and chloroform fractions of the extracts which ranged between 2.1 ppm and 27 ppm. This suggested that crude extracts were more potent than their respective fractions, further explaining that the different fractions of phytochemicals in these plant species work jointly (in synergy) to exert their therapeutic efficacy. Both aqueous and methanol extracts of the two medicinal plants demonstrated a high degree of antioxidant capacity against the DPPH radical with the Duh and Yen inhibition percentage ranging between 4.5% and 72%. Phytochemical studies of the rhizome extracts showed that the major compounds present include flavonoids, tannins, anthocyanidins, anthraquinones, triterpenoids (oleanolic acid), the steroidal saponin Diosgenin, the sugars, rhamnose, glucuronic acid, Arabinose and hexoses. Conclusion: This is the first report of the detection and isolation of diosgenin and oleanolic acid from the rhizome extracts of Ee and Pp. All structures were determined using spectroscopic/spectrometric techniques (1H NMR and 13C and LC-ESI-MS) and by comparison with literature data

Effect of metal poisoning and the implications of gender and age on the elemental composition in patients with mental behavioural disorders

The objective of this work was to investigate the possible correlation between the exposure to selected toxic metals and the behavioural disorder of mentally ill patients. The study also sought to establish if gender and age of the patient had an effect on the pattern of the elemental distribution in their head hair and blood samples. To achieve this, the concentrations of a number of selected toxic metal elements were determined in 60 mentally ill patients and 43 healthy individuals (control) in Ile-Ife area, in Nigeria, using inductively coupled plasma spectrophotometer-optical emission spectrometer (ICP-OES). The behavioural disorder cases investigated were 8 bipolar, 2 post partum psychosis, 43 schizophrenia and 7 non-specific cases. The concentration ranges of Cu, Zn, Ca, Li, V, Be (for both males and females), Cd and Sr (for females only) as analyzed from the patients’ head hair with behavioural disorders, were found to be similar with those of the controls. However, the concentration ranges of Al, Ba, Mg, Cr and Cd, Sr (for males only) were higher in patients than in the controls, while those for K and Fe were found to be higher in the controls than in the patients for both males and females. Blood samples analysis showed that, nearly all the elements were higher in the female (patients and control) than in the males; a possible indication that women may be at greater risk than men. It was also shown that, age may have an influence on the accumulation of some specific elements. The accuracy of the analytical results was experimentally demonstrated by NCS DC 73347 certified reference material that was analyzed along the standards while the significance of the data obtained was tested statistically at both p = 0.01 and 0.05

Determination of antibiotic residues in frozen poultry by a solid-phase dispersion method using liquid chromatography-triple quadrupole mass spectrometry

Importation of poultry produce into Nigeria through its land borders has heightened, notwithstanding the government’s ban on such products. This study examined imported frozen poultry products for antibiotic residues considering their health implications. A solid-phase extraction method using liquid chromatographytandem mass spectrometry in the positive and negative electrospray ionisation and the multiple reaction monitoring modes were employed. The antibiotics were extracted with acetonitrile-dichloromethane. Chromatographic separation was on Waters Acquity UPLC® BEH C18 column with acetonitrile, and water gradient and the antibiotics analysed using Electrospray positive ionisation polarity switch in a single run of fourteen minutes. Residues of nineteen (19) antibiotics were found in the three different matrices at different levels with varying detection frequencies ranging between 2 and 4% (sulfamoxole, penicillin-G, albendazole and phebendazole) and 14–54% for all the other antibiotics. The highest number of violative samples was found in the turkey gizzard and chicken muscle. Sulfixosazole had the highest percentage violation of 80.00% in turkey gizzard while sulfamethoxazole, notwithstanding its lower frequency in chicken muscle had highest maximum concentration and 100% violation. The presence of these drugs, however, does not pose any immediate health risk

Distribution of Antibiotic Residues in Non-medicated Poultry Feeds by High-Performance Liquid Chromatography with Diode-array Detection

This paper reports on the determination and distribution of antibiotic drugs in poultry feeds mainly the layers and growers mash obtained from Ogun state in Nigeria. Pulverized feed samples were initially treated with phosphate buffer adjusted to pH 7 and the analytes extracted in an SPE cartridge with ammonium hydroxide and methanol. The extract reconstituted in phosphate buffer was determined with high-performance liquid chromatography-diode array detection (HPLC–DAD). The analytical column was an XTerra MS C18 column, (4.6 mm x 100 mm, 3.5 μm) with mobile phases consisting of ultrapure water and acetonitrile mixed with 0.1% HCOOH in gradient elution mode. Data acquisition was achieved with AgilentChemStation Version B.040.01 SP1 while the analytes were completely separated under 10 minutes with good resolution and symmetric peaks. The high correlation coefficient (R2) values (> 0.998, excluding sulfadimethoxine) indicate a good correlation between analyte concentration and peak areas. Limit of detection (LOD) and quantitation (LOQ) was between 5.37 and 55.42 ng/g, and 17.91 and 184.74 ng/g, respectively. All the drugs exhibited high mean concentration values in the two feed types, and there was no significant difference between their means (p < 0.05). The results clearly showed that feed millers fortify their feeds with antibiotics mainly sulfonamides in varying amounts without declaring same, thus compromising security of poultry birds and human consumers

Target Analysis of Antibiotic Drugs in Poultry Feedstuff by Solid Phase Extraction and Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

Seventy-five poultry feed samples of two feed types were analysed for antibiotic drugs using a simple generic solid phase extraction procedure with dichloromethaneacetonitrile after delipidation with n-hexane. Analytical separation was performed on a Waters Acquity C18 column with gradient elution consisting of water and acetonitrile. Liquid chromatography–tandem mass spectrometry (LC-MS/MS), with positive and negative electrospray ionization methods in the multiple reaction monitoring modes (MRM), was used for the quantification of 21 compounds from six classes including fluoroquinolones, sulfonamides, lincosamides, anthelmintics, macrolides and the β-lactams in a single chromatographic run of 14 minutes. All the six classes of the drugs were found in the two feed types at concentration ranging between 0.22 – 1505 ng/g. Sulfadimethoxine, sulfaguanidine, sulfamerazine, and sulfamethoxazole were the major sulfonamides in the two feed types with concentration at the part per million levels. Albendazole, penicillin-G, sulfadiazine, sulfaquinoxaline and sulfixosazole were not detected in the layers mash exclusively fed to laying birds; also, sulfamethazine and sulfamozole were the only two drugs not detected in the growers mash meant for birds raised for meat. Ciprofloxacin, sulfadimethoxine, sulfamethoxazole, sulfamerazine, and sulfaguanidine were the most prominent antibiotic drugs in the two feed types. Results from the present study suggest that feed millers surreptitiously fortify their feeds with antibiotics without declaring same, thus exposing poultry chickens to sub-therapeutic dosages of the drugs. It is evident that self-regulation for safety in the poultry industry should be discouraged thus relevant authorities must take steps to reduce and control the use of antibiotics to protect public health

Sensitive and selective electrochemical detection of bisphenol A based on SBA-15 like Cu-PMO modified glassy carbon electrode

This work reports the electrochemical detection of bisphenol A (BPA) using a novel and sensitive electrochemical sensor based on the Cu functionalized SBA-15 like periodic mesoporous organosilica-ionic liquid composite modified glassy carbon electrode (Cu@TU-PMO/IL/GCE). The structural morphology of Cu@TU-PMO is characterized by X-ray powder diffraction (XRD), energy dispersive X-ray analysis (EDX), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), Field emission scanning electron microscopy (FESEM), and Brunauer-Emmett-Teller (BET). The catalytic activity of the modified electrode toward oxidation of BPA was interrogated with cyclic voltammetry (CV) and differential pulse voltammetry (DPV) in phosphate buffer solution (pH 7.0) using the fabricated sensor. The electrochemical detection of the analyte was carried out at a neutral pH and the scan rate studies revealed that the sensor was stable. Under the optimal conditions, a linear range from 5.0 nM to 2.0 mu M and 4.0 to 500 mu M for detecting BPA was observed with a detection limit of 1.5 nM (S/N = 3). The sensor was applied to detect BPA in tap and seawater samples, and the accuracy of the results was validated by high-performance l